Lab Manual-General & Inorganic Chemistry WBU

LAB MANUAL-GENERAL & INORGANIC CHEMISTRY- EXPERIMENTS AND ACTIVITIES
CONTENTS
EXPERIMENTS
1. Lab 1-Rules of technical insurance. Separation of the components of a mixture in several
techniques.
2. Lab 2-Acids, bases and salts
3. Lab 3- Law of conservation of mass
4. Lab 4-Solutions, concentrations of solutions and preparation of solutions in the laboratory.
5. Lab 5-Electrolytic decomposition
6. Lab 6-Chemical equilibrium in electrolyte solutions
7. Lab 7-Hydrolysis of salts and colligative properties
8. Lab 8-Hydrogen, hydrogen peroxide. Oxygen.
9. Lab 9-Halogens.( chlorine and hydrochloride gas)
10. Lab 10-Boron, aluminium, carbon and silicon.
11. Lab 11-Alcaline metals. Magnesium and alkaline earth metals.
12. Lab 12-Oxygenated compounds of nitrogen. Phosphorus.
13. Lab 13-Sulfur gas, sulfuric acid and sulfates, thiosulfates, persulfates.
14. Lab 14-Copper and silver. Zinc, Cadmium, Mercury
15. Lab 15-Iron. Chrome. Manganese.
Literature for students on the development of laboratory classes:
1. "Guide for laboratory work in Inorganic Chemistry": Group of authors, SHBLU 2015 (reprint)
ISBN 99927-0-174-9
2. Jill Robinson, John McMurry, Robert Fay(2020). Chemistry, global edition. Pearson. ISBN-
13 978-0134856230
3. P. Atkins, L. Jones, "Chemical Principles", W.H. Freeman and Company. New York, fourth
edition, 2008 ISBN-13 978-1429209656
MSc. Ergi HOXHA wbu. 2023
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Lab Report Template
Name_______________________
Date of Lab _________________
Title________________________
• Introduction
Begin with background knowledge-What was known before the lab? What is the lab about? Include
any preliminary/pre-lab questions. Also, include the purpose of the lab at the end of the
introduction. Be clear & concise
• Materials
List out the expendables and apparatus in bulleted form (2 columns)
• Procedure
Describe what was performed during the lab
Include diagrams if necessary
If the procedure is taken directly from the lab handout, say so! Do NOT rewrite the procedure!
• Data
Label clearly what was measured or observed throughout the lab
Include all data tables and/or observation
• Calculations
Show work, include units, and clearly label your results
• Analysis
Answer any post-lab questions with complete thoughts. Assume the reader does not know anything
about this topic.
• Conclusions
Refer to the purpose- What was accomplished? Analyze your data, report your findings and
include possible sources of error. How does this relate to topics outside of the classroom?
DO NOT USE PERSONAL PRONOUNS!
(This includes: me, my, I, our, us, they, her, she, he, them, etc.)
THIS LAB REPORT MUST BE TYPED IN ORDER TO RECEIVE CREDIT
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Lab 1-RULES OF TECHNICAL INSURANCE. SEPARATION OF THE COMPONENTS

OF A MIXTURE IN SEVERAL TECHNIQUES.
Lab Safety Rules and Guidelines
We list some of the most common lab safety rules out there, to help you whether you’re
developing or updating a set of policies for your own lab!
Here are the safety rules that most commonly came up in our look at several laboratories’ policies:
General lab safety rules
The following are rules that relate to almost every laboratory and should be included in most safety
policies. They cover what you should know in the event of an emergency, proper signage, safety
equipment, safely using laboratory equipment, and basic common-sense rules.
1. Be sure to read all fire alarm and safety signs and follow the instructions in the event of an
accident or emergency.
2. Ensure you are fully aware of your facility's/building's evacuation procedures.
3. Make sure you know where your lab's safety equipment—including first aid kit(s), fire
extinguishers, eye wash stations, and safety showers—is located and how to properly use it.
4. Know emergency phone numbers to use to call for help in case of an emergency.
6. Lab areas containing carcinogens, radioisotopes, biohazards, and lasers should be properly
marked with the appropriate warning signs. Open flames should never be used in the laboratory
unless you have permission from a qualified supervisor.
7. Make sure you are aware of where your lab's exits and fire alarms are located.
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8. An area of 36" diameter must be kept clear at all times around all fire sprinkler heads.
9. If there is a fire drill, be sure to turn off all electrical equipment and close all containers.
10. Always work in properly-ventilated areas.
11. Do not chew gum, drink, or eat while working in the lab.
12. Laboratory glassware should never be utilized as food or beverage containers.
13. Each time you use glassware, be sure to check it for chips and cracks. Notify your lab
supervisor of any damaged glassware so it can be properly disposed of.
14. Never use lab equipment that you are not approved or trained by your supervisor to operate.
15. If an instrument or piece of equipment fails during use, or isn't operating properly, report the
issue to a technician right away. Never try to repair an equipment problem on your own.
16. If you are the last person to leave the lab, make sure to lock all the doors and turn off all
ignition sources.
17. Do not work alone in the lab.
18. Never leave an ongoing experiment unattended.
19. Never lift any glassware, solutions, or other types of apparatus above eye level.
20. Never smell or taste chemicals.
21. Do not pipette by mouth.
22. Make sure you always follow the proper procedures for disposing of lab waste.
23. Report all injuries, accidents, and broken equipment or glass right away, even if the incident
seems small or unimportant.
24. If you have been injured, yell out immediately and as loud as you can to ensure you get help.
25. In the event of a chemical splash into your eye(s) or on your skin, immediately flush the
affected area(s) with running water for at least 20 minutes.
26. If you notice any unsafe conditions in the lab, let your supervisor know as soon as possible.
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Housekeeping safety rules
Laboratory housekeeping rules also apply to most facilities and deal with the basic upkeep,
tidiness, and maintenance of a safe laboratory.
1. Always keep your work area(s) tidy and clean.
2. Make sure that all eye wash stations, emergency showers, fire extinguishers, and exits are
always unobstructed and accessible.
3. Only materials you require for your work should be kept in your work area. Everything else
should be stored safely out of the way.
4. Only lightweight items should be stored on top of cabinets; heavier items should always be
kept at the bottom.
5. Solids should always be kept out of the laboratory sink.
6. Any equipment that requires air flow or ventilation to prevent overheating should always be
kept clear.
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Dress code safety rules
As you’d expect, laboratory dress codes set a clear policy for the clothing employees should avoid
wearing in order to prevent accidents or injuries in the lab. For example, skirts and shorts might
be nice for enjoying the warm weather outside but quickly become a liability in the lab where skin
can be exposed to heat or dangerous chemicals.
1. Always tie back hair that is chin-length or longer.
2. Make sure that loose clothing or dangling jewellery is secured or avoid wearing it in the first
place.
3. Never wear sandals or other open-toed shoes in the lab. Footwear should always cover the foot
completely.
4. Never wear shorts or skirts in the lab.
5. When working with Bunsen burners, lighted splints, matches, etc., acrylic nails are not
allowed.
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Personal protection safety rules
Unlike laboratory dress code policies, rules for personal protection cover what
employees should be wearing in the lab in order to protect themselves from various hazards, as
well as basic hygiene rules to follow to avoid any sort of contamination.
1. When working with equipment, hazardous materials, glassware, heat, and/or chemicals,
always wear face shields or safety glasses.
2. When handling any toxic or hazardous agent, always wear the appropriate gloves.
3. When performing laboratory experiments, you should always wear a smock or lab coat.
4. Before leaving the lab or eating, always wash your hands.
5. After performing an experiment, you should always wash your hands with soap and water.
6. When using lab equipment and chemicals, be sure to keep your hands away from your body,
mouth, eyes, and face.
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Chemical safety rules
Since almost every lab uses chemicals of some sort, chemical safety rules are a must. Following
these policies helps employees avoid spills and other accidents, as well as damage to the
environment outside of the lab. These rules also set a clear procedure for employees to follow in
the event that a spill does occur, in order to ensure it is cleaned up properly and injuries are
avoided.
1. Every chemical should be treated as though it were dangerous.
2. Do not allow any solvent to come into contact with your skin.
3. All chemicals should always be clearly labeled with the name of the substance, its
concentration, the date it was received, and the name of the person responsible for it.
4. Before removing any of the contents from a chemical bottle, read the label twice.
5. Never take more chemicals from a bottle than you need for your work.
6. Do not put unused chemicals back into their original container.
7. Chemicals or other materials should never be taken out of the laboratory.
8. Chemicals should never be mixed in sink drains.
9. Flammable and volatile chemicals should only be used in a fume hood.
10. If a chemical spill occurs, clean it up right away.
11. Ensure that all chemical waste is disposed of properly.
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Chemistry lab safety rules
As chemistry labs are one of the most common types, these basic chemistry lab safety rules are
relevant to many scientists, dealing with the safe performance of common activities and tasks in
the average chemistry lab:
1. Before you start an experiment, make sure you are fully aware of the hazards of the materials
you'll be using.
2. When refluxing, distilling, or transferring volatile liquids, always exercise extreme caution.
3. Always pour chemicals from large containers to smaller ones.
4. Never pour chemicals that have been used back into the stock container.
5. Never tap flasks that are under vacuum.
6. Chemicals should never be mixed, measured, or heated in front of your face.
7. Water should not be poured into concentrated acid. Instead, pour acid slowly into the water
while stirring constantly. In many cases, mixing acid with water is exothermic.
Electrical safety rules
Like almost every other workplace, laboratories contain electronic equipment. Electrical safety
rules help prevent the misuse of electronic instruments, electric shocks and other injuries, and
ensure that any damaged equipment, cords, or plugs are reported to the appropriate authorities so
they can be repaired or replaced.
1. Before using any high voltage equipment (voltages above 50Vrms ac and 50V dc), make sure
you get permission from your lab supervisor.
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2. High-voltage equipment should never be changed or modified in any way.
3. Always turn off a high-voltage power supply when you are attaching it.
4. Use only one hand if you need to adjust any high-voltage equipment. It's safest to place your
other hand either behind your back or in a pocket.
5. Make sure all electrical panels are unobstructed and easily accessible.
6. Whenever you can avoid using extension cords.
Laser safety rules
Perhaps not as common as some of the other laboratory safety rules listed here, many laboratories
do use lasers and it’s important to follow some key rules of thumb to prevent injuries. In particular,
accidents due to reflection are something that many employees may not think about. A clear set of
rules for the use of lasers is essential to ensure that everyone is aware of all hazards and that the
appropriate personal protective equipment is worn at all times.
1. Even if you are certain that a laser beam is "eye" safe or low power, you should never look
into it.
2. Always wear the appropriate goggles in areas of the lab where lasers are present. The most
common laser injuries are those caused by scattered laser light reflecting either off the shiny
surface of optical tables, the sides of mirrors, or off of mountings. Goggles will help you avoid
damage from such scattered light.
3. You should never keep your head at the same level as the laser beam.
4. Always keep the laser beam at or below chest level.
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5. Laser beams should never be allowed to spread into the lab. Beam stops should always be used
to intercept laser beams.
6. Do not walk through laser beams.
Our Objective
To separate the components of a mixture using the following techniques:
• Separating funnel
• Chromatography
• Centrifugation
• Simple distillation
• Fractional distillation
The Theory
How is a homogeneous mixture different from a heterogeneous mixture?

Most materials in our surroundings are mixtures of two or more components. Mixtures are either
homogeneous or heterogeneous. Homogeneous mixtures are uniform in composition,
but heterogeneous mixtures are not uniform in composition.
Air is a homogeneous mixture and oil in water is a heterogeneous mixture. Homogeneous and
heterogeneous mixtures can be separated into their components by several physical methods. The
choice of separation techniques is based on the type of mixture and the difference in the chemical
properties of the constituents of a mixture.
What are types of separation techniques?
Various types of separation processes are:
• Crystallization
• Filtration
• Decantation
• Sublimation
• Evaporation
• Simple distillation
• Fractional distillation
• Chromatography
• Centrifugation
• Separating funnel
• Magnetic separation
• Precipitation
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Let’s discuss some of the separation techniques

Using a separating funnel:
A separating funnel is used for the separation of components of a mixture between two immiscible
liquid phases. One phase is the aqueous phase and the other phase is an organic solvent. This
separation is based on the differences in the densities of the liquids. The liquid having more density
forms the lower layer and the liquid having less density forms the upper layer.
Applications:
• To separate a mixture of oil and water.

• To separate a mixture of kerosene oil and water.
Chromatography:
Chromatography is a separation technique used to separate the different components in a liquid
mixture. It was introduced by a Russian Scientist Michael Tswett. Chromatography involves the
sample being dissolved in a particular solvent called mobile phase. The mobile phase may be
a gas or liquid. The mobile phase is then passed through another phase called stationary phase.
The stationary phase may be a solid packed in a glass plate or a piece of chromatography paper.
The various components of the mixture travel at different speeds, causing them to separate. There
are different types of chromatographic techniques such as column chromatography, TLC, paper
chromatography, and gas chromatography.
Paper chromatography is one of the important chromatographic methods. Paper chromatography
uses paper as the stationary phase and a liquid solvent as the mobile phase. In paper
chromatography, the sample is placed on a spot on the paper and the paper is carefully dipped into
a solvent. The solvent rises up the paper due to capillary action and the components of the mixture
rise up at different rates and thus are separated from one another.
Applications:
• To separate colors in a dye.

• To separate pigments from natural colors.
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• To separate drugs from the blood.
Centrifugation:
Sometimes the solid particles in a liquid are very small and can pass through a filter paper. For
such particles, the filtration technique cannot be used for separation. Such mixtures are separated
by centrifugation. So, centrifugation is the process of separation of insoluble materials from a
liquid where normal filtration does not work well. The centrifugation is based on the size,
shape, and density of the particles, viscosity of the medium, and the speed of rotation. The principle
is that the denser particles are forced to the bottom and the lighter particles stay at the top when
spun rapidly.
The apparatus used for centrifugation is called a centrifuge. The centrifuge consists of a centrifuge
tube holder called rotor. The rotor holds balanced centrifugal tubes of equal amounts of the solid-
liquid mixture. On rapid rotation of the rotor, the centrifuge tubes rotate horizontally and due to
the centrifugal force, the denser insoluble particles separate from the liquid. When the rotation
stops, the solid particles end up at the bottom of the centrifuge tube with liquid at the top.
Applications:
• Used in diagnostic laboratories for blood and urine tests.

• Used in dairies and home to separate butter from cream.
• Used in washing machines to squeeze water from wet clothes.
Simple distillation:
Simple distillation is a method used for the separation of components of a mixture containing two
miscible liquids that boil without decomposition and have sufficient differences in their boiling
points.
The distillation process involves heating a liquid to its boiling points, transferring the vapors into
the cold portion of the apparatus, then condensing the vapors and collecting the condensed liquid
in a container. In this process, when the temperature of a liquid rises, the vapors pressure of the
liquid increases. When the vapor pressure of the liquid and the atmospheric pressure reach the
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same level, the liquid passes into its vapor state. The vapors pass over the heated portion of the
apparatus until they come into contact with the cold surface of the water-cooled condenser. When
the vapor cools, it condenses and passes down the condenser and is collected into a receiver
through the vacuum adapter.
Applications:
• Separation of acetone and water.

• Distillation of alcohol.
Fractional distillation:
Fractional distillation is used for the separation of a mixture of two or more miscible liquids for
which the difference in boiling points is less than 25K. The apparatus for fractional distillation is
similar to that of simple distillation, except that a fractionating column is fitted in between the
distillation flask and the condenser.
A simple fractionating column is a tube packed with glass beads. The beads provide surface for
the vapors to cool and condense repeatedly. When vapors of a mixture are passed through the
fractionating column, because of the repeated condensation and evaporation, the vapors of the
liquid with the lower boiling point first pass out of the fractionating column, condense and are
collected in the receiver flask. The other liquid, with a slightly higher boiling point, can be
collected in similar fashion in another receiver flask.
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Applications:
• Separation of different fractions from petroleum products.

• Separation of a mixture of methanol and ethanol.
Learning outcomes
1. Student understands the following terms: solvent extraction, chromatography, RF,

centrifugation, simple distillation, fractional distillation, etc.
2. Student acquires skills to perform experiments using the following techniques in the chemistry
lab:
• Solvent extraction using separating funnel
• Paper Chromatography
• Centrifuge machine
• Simple distillation & fractional distillation
3. Students can identify the components in the mixture based on the knowledge of Rf value,
boiling point, density, etc.
4. Student is able to select & design the above techniques based on the chemical and physical
properties of the components in the mixture.
5. Students acquire the skill arrange the requirements for each technique through the animations,
simulators and videos.
6. Students will be able to select and perform suitable separation techniques based on the
available information about the nature of the components in the mixture.
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Lab-2 - ACIDS, BASES AND SALTS

Acids contain hydrogen in their molecule, which can be replaced by metals by treating salts. Acid
solutions have an acrid taste and turn blotting paper red. Based on the number of hydrogen atoms
that are in a molecule and that can be replaced by metals, we distinguish monobasic acids (for
example HNO3); dibasic (eg H2SO4) etc. Most acids contain oxygen in their molecular
composition. These acids are called oxyacids, e.g. HNO3). Acids that do not contain oxygen are
called hydracids (for example HCI). It is characteristic of the structure of oxyacid molecules that
The first method can serve to produce only hydracids (oxygen-free acids). The second method
serves to produce only oxyacids (acids with oxygen). The third method serves to produce both
oxyacids and hydracids. This method is usually used to produce volatile acids or acids that are
difficult to dissolve.
Bases contain in their composition hydroxyl (oxidril) OH groups that can be replaced by acid
radicals forming salts. In base molecules, the hydroxyl groups (oxidrils) are connected to the metal
atom
For example:
Most bases are not soluble in water.

Acids can be produced in the following ways:
1) By combining some metalloids with hydrogen and then dissolving the extracted product in
water; for example, during the merger of. chlorine with hydrogen produces hydrochloric gas,
which, being dissolved in water, forms hydrochloric acid.
2) By combining acid oxides (anhydrides) with water, e.g.
3) Through the interaction of salt with acid, e.g.:
dibasic (eg H2SO4) etc. Most acids contain oxygen in their molecular composition. These acids
are called oxyacids, e.g. HNO3). Acids that do not contain oxygen are called hydracids (for
example HCI). It is characteristic of the structure of oxyacid molecules that
Bases that dissolve in water are called alkalis. Alkali solutions give litmus a blue color, while
phenolphthalein gives a red color.
Bases can be prepared (produced) in the following ways:
1. From the combination of basic oxides (of metals) with water) e.g.:
2) By the interaction of metals with water; for example:
3) By the interaction of salts with an alkali; for example:
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The first two methods are used to produce alkaline earth metal bases, whose solubility in water is
quite large. The third method can be used to produce both soluble and water-insoluble bases.
In industry, other methods are also used for the production of acids and bases. Thus, for example,
nitric acid is produced by ammonia oxidation, while sodium hydroxide is produced by electrolysis
of aqueous solution of NaCl.
Apparatus and containers:
1) technical-chemical scale with weight box; 2) measuring cylinder with 50 ml pupil; chemical
glass beaker, 3) glass container with pupil 500 ml; 4) large crystallizers; 5) funnel, 6) iron spoon
for burning; 7) glass birch; 8) test tube holder 9) test tube.
Reagents and materials: 1) calcium; 2) magnesium (powder); 3) sulfur; 4) magnesium oxide
MgO; 5) calcium oxide CaO (in pieces); 6) phosphoric anhydride P2Os; 7) calcium hydroxide Ca
(OH)2; 8) sodium acetate CH3COONa; 9) litmus paper; 10) filter paper; 11) pieces of nappe (thin
fabric).
Solutions: 1) sulfuric acid H2SO4 (1:5); 2) hydrochloric acid HCI (2 normal); 3) sodium
hydroxide NaOH (2 normal); 4) sodium carbonate Na2CO3(10%); 5) magnesium sulfate MgSO4
(0.5 normal); 6) copper sulfate CuSO4 (0.5 normal); 7) ferric chloride FeCl3 (O.5 normal); 8)
enticing (turnisol); 9) phenolphthalein (alcoholic); 10) methyl orange.
Practical work
1. Combining anhydride with water
a) Take some phosphoric anhydride with a glass rod and mix it with a small amount of water. Test
the solution produced with blue litmus paper. Note the color change of the lure. Write the reaction
equation.
b) Pour 2-5 ml of water into a large (200-400 ml) glass container. Heat some flowers of sulfur in
an iron spoon until it catches fire, then immerse the spoon in the container (with a little water)
covering it with a watch glass or glass plate. After the sulfur has burned, take out the spoon and
shake the contents of the container, adding a few drops of the solution of the blue beaker. Notice
the change in the color of the beaker. Write the equations of the reactions.
2. Hydrogen bonding with the metalloid.
Pour a small amount of solid sodium acetate into a test tube and wet this with dilute sulfuric acid.
Smell for the presence of acetic acid. In the mouth of the test tube insert, without touching its sides,
a blue tracing paper moistened with water. Note the colour change of the lure. Write the reaction
equation.
3. Combining basic oxide with water
Pour 4-5 ml of water and some magnesium oxide (powder) into a test tube. Close the mouth of the
test tube on the ball of the finger and then shake (the test tube). With a test tube, add 2-3 drops of
the solvent or phenolphthalein. Observe the colour of the contents of the test tube. Write the
reaction equation. In a porcelain glass, wet some pieces of quick lime with water. Note the release
of heat and the pulverization of the lime pieces. Shake a portion of the powder in a test tube with
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a quantity of distilled water. Test the obtained solution with a red stain with phenolphthalein. Write
the reaction equation.
4. Interaction of metal with water
a) Wrap a small amount of metallic calcium in cheesecloth and bring it under the test tube filled
with water, which is inverted in a glass of water. Collect the released gas in a test tube. Take the
gas-filled test tube out of the water by holding it vertically with the mouth down. Prove that this
gas is hydrogen. For this, place a lighted match under the mouth of the test tube. The gas will burn.
Note the formation of a white cloud in the beaker. Pour a few drops of phenolphthalein into the
contents of the glass. Look at the display of red. Write the equation for the reaction that takes place
between water and calcium.
b) Pour 5 ml of distilled water and some magnesium powder into a test tube. Heat the test tube for
3-5 minutes and then add 1-2 drops of phenolphthalein. Note the appearance of red color, write
5. The interaction of salt with alkalis
a) Pour NaOH solution into the test tubes containing the solutions of MgSO4, FeCl3 and CuSO4
salts. Note the formation of precipitates and note their colors. Write the reaction equation.
b) Pour 60 ml of 10% Na2CO3 and 5 Ca(OH)2 into a porcelain container. Boil the contents of the
container by adding water so that the volume of the contents of the container remains unchanged
during boiling. Continue heating until the Na2CO3 is completely reacted. To test this, take a small
portion of the solution and filter it. Add hydrochloric acid to the filtrate until the acid reaction. If
the Na2CO3 has entered the reaction completely, then no bubbles of carbon dioxide will come out
during the throwing of the acid. Write the reaction equation and indicate which substance is in the
filtrate and which in the precipitate.
Salt Production
Types of salts can be simple: normal, acidic, double basic and complex.
Normal salts are products of complete replacement of the acid hydrogen by a metal. We can
consider the molecules of normal salts to be composed of metals and acid radicals.
Normal salts can be produced by the interaction of: 1) a metal with a metalloid, 2) a metal with an
acid. 3) of a basic oxide with an acid; 4) of a metal with the salt of another metal; 5) of a basic
oxide with an anhydride (acidic oxide, 6) of an anhydride with a base; 7) of an acid with a base;
8) of a salt with an acid; 9) of a salt with a base; 10) of a salt with another salt.
The last three ways can be used for the practical knowledge of salts, only in those cases when the
reaction products come out in gaseous or precipitate form. This is something that the reaction is
known and go to the end.
So for example, if we take KCl and MgSO4, the reaction will not be greater, because both salts
that would be formed (K2SO4 and MgCl2) are also soluble in water.
After evaporation to the bottom of the solution of the two initial salts (KCl and MgSO4) the
influence of the 4 salts will crystallize. To separate them is too much trouble.
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On the contrary, during the interaction of BaCl2 with K2SO4, the reaction not only goes to the
end, because one (BaSO4) before the salts that are formed is practically insoluble (hardly soluble)
in water.
In this case, the produced salts are easily separated from each other by filtration.
Acid salts, from the point of view of composition, are products of the partial replacement of
hydrogen of the acid by the metal. In composition. of the acid salt molecule, in addition to the
metal and the acid radical, hydrogen also enters, which can be replaced by a metal, e.g. NaHSO4,
Ca(HSO4)2.
Acid salts can be produced:
1) From the interaction of a base with an acid, the latter is obtained
NaOH+H2SO4=NaHSO4+H2O
NaOH+H2SO4=NaHSO4+H2O
2) From the interaction of normal salt with acid:
Na2SO4+H2SO4=2NaHSO4
Basic salts, from the point of view of composition, are products of the partial replacement of
hydroxyls (oxides) of bases by acid radicals. In the composition of the molecule of a basic salt, in
addition to meta and the acid radical, there are also hydroxyl groups, for example Mg(OH)CI, Bi
(OH)2NO2.
Basic salts can be produced:
1. From the interaction of an acid with a base (the latter with excess):
HC1+Mg (OH)2 = Mg(OH)Cl+H2O
2. From the reciprocal action of a normal salt with a base:

Bi(NO3)3+2NaOH=2NaNO3+Bi(OH)2NO3
Apparatus and containers

1. technical-chemical scale and weight box;
2. Kip's apparatus filled to cook CO2.
3. tripod with ring;
4. Lamp;
5. iron plate
6. measuring cylinder with 25 ml pupil
7. large crystallizers;
8. glass birch;
9. test tube holder;
Reagents and materials: 1)zinc (granule and powder) 2) sulfur (powder); 3) lead oxide PbO; 4)
litmus paper; 5) birch wood.
Solutions: hydrochloric acid HCI (2 normal); 2) sodium hydroxide NaOH (2 normal); 3) barite
water Ba(OH)2 (saturated); 4) barium chloride BaCl2 (1 normal); 5) Ferric chloride FeCl3(0.5
normal) 6) Silver nitrate AgNO3(0.1 normal); 7) barium nitrate Ba(NO3)2 (1 normal); 8)
potassium sulfate K2SO4 (1 normal); 9) magnesium sulfate MgSO4 (1 normal); 10) copper sulfate
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CuSO4 (0.5 normal); 11) lead acetate Pb(CH3 COO)2(0.5 normal)from the undissolved part of
the lead oxide, pouring (pouring) it into another test tube. As the liquid cools, note the separation
of white crystals of lead chloride. Write the reaction equation.
Practical work
1. Union of metal with metalloid
Calculate the amount of sulfur needed to combine with 0.5 grams of zinc to cook (produce) zinc
sulfide. Weigh on the technical-chemical scale 0.5 grams of zinc powder and the corresponding
amount of sulfur powder. Mix the zinc with the sulfur on an iron plate placed on the tripod ring
inside the fume cupboard. Ignite the mixture with a lit birch (pine) stick. Careful! look through the
low glass of the fume hood. Note the ignition and the formation of the white powder of zinc sulfide.
Pour a portion of zinc sulphide into a test tube and then add dilute hydrochloric acid.
Note the release of hydrogen sulfide gas that smells like rotten eggs. Therefore, zinc sulfide is the
salt of hydrogen sulfide. Write the equations of the reactions.
2. Interaction of the basic oxide with the acid
Pour a small amount (about 0.5 g) of lead oxide and 2-3 ml of dilute hydrochloric acid into a test
tube. Heat this mixture until it boils for a few minutes. Separate the juice from the undissolved
part of the lead oxide, pouring (pouring) it into another test tube. As the liquid cools, note the
separation of white crystals of lead chloride. Write the reaction equation.
3. Interaction of the anhydride with the base
Pour a small amount of barium hydroxide solution (barite water) into a test tube and bubble a
stream of carbon dioxide through it. Note the separation of the white precipitate.
4. Interaction of the acid with the base
Pour into a porcelain beaker 10 ml, 2 normal solution of HCI and add little by little 2 normal
solutions of NaOH. Each time you add NaOH, stir the contents of the beaker with a glass rod and
test its reaction on the litmus test. For this, with the side of the glass rod, take a drop of the solution
and meet the litmus paper. You will continue adding NaOH until the beaker's dissolution reaction
becomes neutral.
Such digestion does not change the color of the lure. If no solution is obtained, evaporate to a dry
residue. Taste the salt produced. Write the equation
5. Interaction of the metal with the salt of another metal
Pour 5-6 ml of copper sulfate solution (CuSO4) and 2-3 grains of zinc into a test tube. Heat the
contents of the test tube by stirring until it boils. Continue mixing until the solution becomes
colorless. Note the formation of metallic copper. Filter the solution and collect the filtrate in a
porcelain cup. Cool the filtrate in a water bath. Note the separation of colorless crystals of zinc
sulfate ZnSO4. 7H2O. Write the reaction equation.
6. Interaction of salt with an acid
21
In a test tube, mix a small amount of silver nitrate solution AgNO3 with dilute hydrochloric acid.
Note the separation of a white hair-like precipitate. Write the reaction equation.
7. The interaction of the salt with the base
Pour ferric chloride FeCl3 solution and sodium hydroxide solution into a test tube. Note the
separation of the brown to red precipitate. Table salt remains in digestion. Test this by evaporating
the filtered solution. Write the reaction equation.
8. Interaction between two salts
a) In a test tube containing a solution of barium chloride BaCl2, pour the solution of potassium
sulfate K2SO4
b) Pour barium nitrate solution Ba(NO3)2 and magnesium sulfate solution MgSO4 into a test tube.
In both cases, notice the formation of a white precipitate of BaSO4. Write the equations of the
reactions.
9. Preparation of acid salt

Pour 3-4 ml of barite water, Ba(OH)2, into a test tube and bubble a stream of carbon dioxide
through it. Note the separation of the white precipitate of BaCO3. Continue bubbling carbon
dioxide until the precipitate is completely dissolved. The dissolution of the precipitate is caused
by the formation of the acid salt, barium hydrogen carbonate Ba(HCOз)2 which is soluble in water.
Write the equations of the reactions.
10. Preparation of basic salt
a) Pour copper sulfate solution into a test tube and add excess NaOH solution. Note the formation
of blue colored amorphous precipitate of Cu(OH)2. Heat the sample. Note the darkening of the
precipitate, due to decomposition of Cu(OH)2, into black cupric oxide and water.
In a second test tube again pour copper sulfate solution and sodium hydroxide solution, but this
time the amount of NaOH solution is smaller (almost half of the first one). Reheat the liquid
together with the precipitate that forms. This time the color change of the precipitate will not occur,
because this is no longer the hydroxide, but the basic copper sulfate Cu2(OH)2SO4.
Write the reaction equation for the formation of this salt.
b) Pour some lead oxide into a test tube containing lead acetate solution and heat the test tube.
Note the formation of a white precipitate of the basic salt of basic lead acetate Pb(OH) (CH3COO).
Write the equation for the reaction.
Lab 3- LAW OF CONSERVATION OF MASS
One of the fundamental laws of chemistry and physics is the law of conservation of mass of the
substance.
The wording of this law, in general, today is done in this way:
"The weight (mass) of the substances entering the reaction is equal to the weight of the substances
leaving the reaction".
This law has been of great importance for chemistry because it is the basis of the entire theory on
chemical transformations of substances. Relying on this law, chemists do the calculations and
22
check the accuracy of the studies done by them, because the lack of equality between the weight
of substances received and the weight of substances produced shows that the study is not regular.
The law of conservation of the mass of the substance entered those laws that are used every day in
laboratory practice, as well as in industrial practice.
1. technical-chemical scale (or commercial scale)
2. licking with the pupil 400-500 ml
3. rubber tube with a length of 12-15 cm
4. fasten
5. tools for catching the combustion products (wire triangle with a net on it, lamp socket filled with
sodium hydroxide, according to figure 46).
6. candle.
Reagents and materials
1. iron (powder)
2. sodium hydroxide (copra or cane)
Practical work
1. Oxidation of metals in closed containers
Pour half a spoon (laboratory) of iron powder into a 400-500 ml student lick. At the end of the
lick, pipe put a piece of rubber pipe with a length of 12-15 cm (fig. 45). Tighten this funnel at a
distance of 2-3 cm from its end with a Mohr clamp and then weigh the lick with an accuracy of up
to 0.01 gram.
Heat the lick together with the iron powder. At first, heat it very carefully and by rocking it
(licking) so that the powder is constantly in motion. Cool the shell and reweigh it with the same
precision. You will notice that the weight of the lick before and after heating will have remained
unchanged.
Carefully open the clamp and notice how air rushes into the lick. Reweigh the lick again.
Why did its weight increase?
How to write reviews:
1. lick weight before and after gi heat
2. the weight of the lick after the air enters it g2
23
3. increase in weight as a result of the crushing of metal g2-g1
2. Combustion and absorption of combustion products
Prepare a wire triangle with a net and a bulb socket. Balance the apparatus built in this way and
then light the candle. After a few minutes, you will notice that the plate in which the candle is
located will become heavier. Explain why the equilibrium is broken? After finishing the
experiment, pour the sodium hydroxide into its container, to use it in future experiments.
Lab 4- SOLUTIONS, CONCENTRATIONS OF SOLUTIONS AND PREPARATION OF

SOLUTIONS IN THE LABORATORY
A solution is a homogeneous system composed of two or more substances, where one (or
several) substances is dissolved, that is, it is uniformly distributed in the other, that is, in the
solvent. As a solvent, usually, the substance that is in the solution in the largest amount is taken.
In the case of aqueous solutions, the solvent is water.
The dissolution of substances is accompanied by heat release (positive thermal effect), or heat
absorption (negative thermal effect) and volume changes. These phenomena, as well as some
others, depending on the mutual chemical action of the dissolved substance with the solvent.
During the dissolution process, the particles of the dissolved substance form with the molecules
of the solvent-defined compounds, which are called solvates. Solvates are generally less stable. In
cases where water is the solvent, the solvates are called hydrates. Solvates form more easily and
are more stable the more polar the molecules of the solute and solvents.
Sometimes the water molecules are so strongly bound to the particles of the dissolved substance
that the latter separates from the solution in the form of crystals, in the composition of which water
also enters. These crystals, which contain water in their composition, are called crystal hydrates,
while the water contained in them is called water of crystallization.
During the digestion of solid substances, two processes take place. In the first process, the
particles of the substance in the solution are distributed, which is accompanied by heat absorption;
while in the second, the formation of hydrates occurs, which is accompanied by the release of heat.
Depending on the type of process that prevails, the overall thermal effect of digestion will be
positive or negative.
Knowing the heat of dissolution of the anhydrous salt (without water) and that of its crystal
hydrate, the heat of hydration (of combining with water molecules) can be calculated.
The calculations, in this case, are made on the basis of the basic law of thermochemistry, which
states that the thermal effect of a chemical reaction does not depend on its path, but on the initial
and final state of the substances that participate in the reaction
Practical Work
24

1) technical-chemical scale with weighing box, 2) barometer; 3) thermometers (up to 150℃) and
room thermometer; 4) stand with rings and clips; 5) corks; 6) apparatus to determine the solubility
of air in water according to figure 55 (stand with ring and clamps, lamp, jar with 200-250 ml pupil;
glass crystallizer, test tube with rubber ring and stopper with funnel for air extraction); 7)
measuring cylinders with 100 and 250 ml student; 8) metal crystallizer, 9) mortar with 100 ml
student 2 pieces and 200 ml student; 13) separating funnel; 14) funnels 2 pieces; 15) bottles for
collection of solutions; 16) burette; 17) tweezers; 18) horn spoon; 19) test tube holders; 20) small
test tubes with stoppers and rubber rings; 21) asbestos nets; 22) glass rods; 23) samples.
1) potassium hydroxide KOH, 2) ammonium nitrate NH4NO3; 3) potassium nitrate KNO3, 4)

potassium dichromate K2Cr2O7; 5) sodium thiosulfate Na2S2O3. 5H2O; 6) sodium sulfate
Na2SO4. 10 H2O; 7) sodium acetate CH3COONa. 3H2O;8)sodium chloride NaCl; 9) anhydrous
copper sulfate CuSO4; 10) copper sulfate crystal hydrate CuSO4. 5 H2O. 11) ether C4H1oO; 12)
filter paper; 13) cotton; 14) birch wood.
Solutions: 1) calcium acetate Ca(CH3COO)2 (saturated)
1. Heat of digestion
Pour (up to 1/4) water into two test tubes and measure its temperature. In the first test tube, pour
0.5-1 gram of ammonium nitrate, mix carefully with the thermometer and mark the lowest
temperature. In the second test tube, connect a few pieces of potassium hydroxide and after mixing,
record the highest temperature. What thermal effect is observed during the digestion of these
substances?
2. Volume change during digestion
Pour in a sample of water (up to 1/3) and then carefully add an equal volume of alcohol. Fix (mark)
the upper level. of the liquid by means of a rubber ring. Close the test tube with a cork and mix
with cayenne. After cooling, notice the decrease in the level of digestion. Explain why this
happens.
3. Determining the degree of salt solubility
Weigh 10-12 grams of finely crushed potassium nitrate on a technical-chemical scale and dissolve
it in a container with 25 ml of water, heating the mixed vinegar as well. Then cool the vessel with
water to laboratory temperature. What will the prepared digestion be called? Filter the solution
through a dry filter paper. Collect the filtrate and measure the temperature.
Weigh a dry porcelain cup, pour into it about 10 ml of nitrate (solution) and weigh again. Carefully
heat the flask with the solution on an asbestos grid, covering the flask with a weighted funnel.
(Why?) Continue heating until all the water evaporates and the funnel remains dry. After cooling,
wash the cup and the funnel again. How can you check that all the water has evaporated?
25
Processing of conclusions
The calculation is done starting from the experimental data:
a) the weight of the solution taken for evaporation;
b) weight of dry salt contained in 10 ml of solution.
c) weight of water contained in 10 ml of solution;
d) the solubility of potassium nitrate by expressing it in g/100g of water as well as in g/100g of

solution for the measured temperature (of the filtrate).
Based on the data in table 4 (see appendices at the end), construct the solubility curve of KNO3.
Using the constructed curve, find the solubility of KNO3 for the temperature measured during the
experiment (filtrate) and compare it with the value found experimentally.
4. Dependence of the solubility of salts on temperature
a) Pour water into a test tube and add to it a small amount of powdered potassium dichromate and
shake the test tube until the salt is completely dissolved. Add KzCr2O, and shake the test tube
again until a little dissolved salt remains at the bottom. Heat the test tube until the salt dissolves
and again continue to add K2Cr2O7 to the hot solution until the saturated solution is reached (at
the bottom of the test tube undissolved crystals should remain.) The solution is heated to boiling
and then allowed to cool to the temperature of the laboratory.
What is the solubility of K2Cr2O in cold water and in hot water? b) Pour water into a test tube and
then add some table salt. Dissolve the salt by heating it. If the salt is all dissolved, continue to add
more until it becomes saturated. Separate the hot solution from the undissolved crystals in another
test tube and let it cool. Note the formation of a small amount of salt crystals. Explain the results
of the experiment using the data on the solubility of NaCl (table 5).
c) Pour saturated solution of Ca(CH3COO)2 into a test tube and heat it. Note the formation of
crystals. Explain the conclusion of the experiment.
5. Oversaturated digestions
a) Pour 5 grams of sodium acetate and 3 ml of water into a test tube. Heat the sample until all the
salt is dissolved. Then close the mouth of the test tube with a piece of cotton and place (the test
tube) in a glass of cold water. When the solution has cooled, remove the cotton and drop a small
crystal of sodium acetate into the test tube. Immediately around the latter, crystals begin to grow,
which quickly harden the contents of the test tube. Focus on releasing heat.
b) Heat a small amount of sodium thiosulfate crystal hydrate in a test tube. At 48°C these crystals
are completely dissolved in the water of crystallization and form supersaturated solutions of
Na2S2O3. Cool this solution carefully with tap water and then drop into it a small crystal of
thiosulphate. Note the solidification of the entire solution into a crystalline mass as well as the
release of heat.
26
Only by heating do you redissolve the crystals in the test tube. After cooling the sample with water,
rub it with a glass rod on its inner sides that are wet from the solution. Note the crystallization of
the solution again.
6. Properties of crystal hydrates
a) Pour a small amount of copper sulfate crystal hydrate (blue stone) into a test tube. Fix the test
tube on the tripod so that its end is slightly higher than the nozzle (Why)? Heat the sample. Note
the color changes of the crystals. Stop heating when all the obtained substance turns white. After
cooling the test tube, pour 2-3 drops of water into it. Focus on the release of heat and the color
change. Write the equations of the reactions.
b) Heat a small amount of sodium thiosulfate crystal hydrate in a test tube. At 48°C these crystals
dissolve. Continue heating until the solid salt remains. After cooling the test tube, pour a few drops
of water into it. Note the heating of the test tube. Write the equations of the reactions.
7. Dissolving the anhydrous salt and its crystal hydrate
a) Weigh about 10 grams of Glauberi salt. Pour 10 ml of water into a chemical beaker and measure
its temperature. Without removing the thermometer from the water, pour the weighed salt into it
and mix the solution with the thermometer. Focus attention on the digestion temperature. Record
the temperature of the water and that of the digester.
b) Weigh about 10 grams of Glauber's salt and crush it in a porcelain cup, mixing it with a glass
rod. The salt first dissolves in the water of crystallization, which evaporates with further heating.
Write the reaction equation.
After cooling, crush the crushed salt in a mortar and pour it into a chemical beaker containing 10
ml of water, the temperature of which has been measured before. Note the temperature change.
Record the temperature of the water and digester. Explain the difference in the thermal effect of
dissolution of Glauber's salt and anhydrous sodium sulfate.
Based on the data in Table 5 (see appendices at the end), draw the conclusion about the change in
the solubility of Na2SO4 and 80
Na2SO4. 10 H2O with increasing temperature. What relationship can you note between the
thermal effect of dissolution and the change in solubility with temperature?
8. Determination of water of crystallization
Weigh a pot or a porcelain cup on the technical-chemical scales with an accuracy of up to 0.01 g.
Then weigh into it, with the same precision, about 1 g of finely ground copper sulfate crystal
hydrate. Place the pot (or cup) on the ring of a stand equipped with asbestos mesh and heat
carefully until all the salt is white. After the pot (or cup) has cooled in the desiccator, weigh it
again. Repeat the heating and weighing to ensure complete removal of water from the salt.
1) Starting from the data of the experiment, calculate:
27
a) the weight of the salt taken,
b) the weight of the salt after crushing;
c) the weight of the water of crystallization,
ç) the amount in grams of water corresponding to one gram-molecule of CuSO4;
d) the number of gram-molecules of water of crystallization, corresponding to one gram-molecule

of CuSO4.
2) Write the formula of cupric sulfate crystal hydrate.
9. Cleaning of salts
a) Pour about 10 grams of potassium nitrate and about 0.1 gram of copper sulfate into a chemical
beaker. Add 10 ml of water and heat the glass to dissolve the salts. Cool the warm solution by
placing the beaker in a bath of cold water and stirring the solution with a glass rod. Note the
formation of a large quantity of small, colorless crystals of KNO3. Copper sulfate remains in the
solution. What's her name? Explain why saltpeter crystallizes, while copper sulfate remains in
solution.
Filter the formed crystals, rinse them on the filter with a small amount of water and dry them by
pressing them between sheets of filter paper. Weigh the dried crystals and calculate their weight.
What properties of dissolved substances are based on their purification by crystallization? Can all
substances be purified by crystallization?
b) Dissolve in 100 ml of water by heating 20-25 grams of table salt mixed with copper sulfate.
If the solution is cloudy, filter it. Evaporate the solution in a porcelain cup until 1/3 of the original
volume remains. Table salt crystals will form, while copper sulfate will remain in solution. Filter
the NaCl crystals, rinse them with a small amount of water and then dry them by pressing them
between sheets of filter paper. Weigh the dried crystals and calculate their amount. Is it reasonable
for table salt to be purified by recrystallization and for the purification of which substances is
vaporization required?
10. Solubility of liquids in water
a) Pour 2-3 ml of glycerin into a test tube and carefully add an equal amount of water. Two layers
will form. Mix the liquids well. Note their complete digestion.
b) In a separatory funnel pour 4-5 ml of water and the same amount of ether (this work is done
away from the fire). Close the funnel with a stopper, shake this mixture well and then let it settle.
Two layers will form. Above will be the solution of water in ether, while below will be the solution
of ether in water. After removing the cork with a pipette, take the liquid (digestion) in a test tube;
of the bottom layer. Pour the remaining (top) ether layer into a dry test tube through the mouth of
the separatory funnel.
28
To test the presence of ether in the water layer (bottom), carefully heat the liquid of the first test
tube. Place a lit match near the mouth of the test tube. Note the flash of vapor coming from the test
tube. Pour a little bleached copper sulfate (anhydrous) into the ether layer. The partial blue coloring
of the latter due to the formation of copper sulfate crystal hydrates indicates the presence of water
in the ether.
On the basis of the last two experiments draw a conclusion about the mutual solubility of liquids.
Give an example of two liquids that are practically insoluble in each other.
11. Solubility of air in water
Build the apparatus according to figure 55. In the pot with the 200-250 ml student, the glass tube,
which serves to remove the gas, should not be inserted deeper than the stopper. Its end should be
level with the end of the cork. Try kissing (sealing) the device. Pour water into the pot until it
meets the bottom of the inserted cork. Measure the volume of pot water with the side of a cylinder
82
large meter. Then fill the pot and the gas extraction pipe with water from the tap (waterworks).
Heat the water in the pot until it boils for a few minutes. Collect the released air in a graduated
funnel with a bottom (large sample) and filled with water (as shown in the picture). When all
dissolved air has been released, remove the degassing tube from the water and stop heating.
After cooling, adjust the surface of the water in the crystallizer and in the graduated tube (test tube)
so that they are on the same level. Do this by plunging the graduated funnel deeper into the
crystallizer water. Measure and record the volume of air released, the temperature of the water and
the atmospheric pressure
1. Calculate the density of the air collected above the water. The water vapor plot for the laboratory
temperature during the experiment can be found in Table 2 (cf. appendices at the end).
2) Find the volume of air dissolved in water under normal conditions.
3) Calculate the volume (measured under normal conditions) of dry air dissolved in 100 ml of
water under the conditions of the experiment.
4) Compare the conclusion drawn with that found in Table 3 (see appendices at the end) and
explain the reasons for the discrepancy.
Preparation of Solutions
The amount by weight or volume of solute contained in a certain amount (weight or volume) of
the solution is called concentration. If the amount of dissolved substance refers to a certain weight
of the solution, then it is called weight concentration, but if it refers to the volume of the solution,
then it is called volumetric. Weight concentration is usually expressed as a percentage or
characterized by the specific gravity of the digestate. The volumetric concentration is expressed
29
by the degree of molarity or normality, the weight of the dissolved substance is expressed
respectively in gram molecules or in gram-equivalents per liter of solution.
a) Percentage concentration of the solution:
It shows the number of grams of dissolved substance in 100 grams of solution. For example, the
10% solution of table salt is that solution in which 100 grams contain 10 grams of salt and 90
grams of water.
b) Preparation of percentage solutions.
To prepare a certain amount of solution with a given percentage concentration, first calculate the
weight of the substance to be dissolved and then the weight of the solvent. If the substance to be
dissolved is taken in the form of crystal hydrate, then during the preparation of the solution, the
concentration of which is calculated on the basis of the anhydrous substance (without water); you
must consider water of crystallization.
c) The molar concentration is expressed by the number of gram-molecules of dissolved

substance in one liter of solution.
The solution containing 1 gram-molecule of the dissolved substance in one liter is called
monomolar or molar and is denoted by 1 M. If the solution contains 0.1 gram-molecule in 1 liter,
then this is called one-tenth-molar (decimolar). and is marked with 0.1 M, etc.
d) Preparation of solutions.
To prepare a certain volume of solution with a certain molarity, first, calculate the weight of the
substance to be dissolved. Weigh the substance on an analytical scale, then dissolve it in a glass
with the smallest (minimal) amount of distilled water. Pour the dissolved substance without a loss
(quantitatively) into the measuring pot with the corresponding student. After that, fill the
measuring cup with distilled water up to the mark and mix the solution well.
If you will prepare the solution from the crystal hydrate, then during the calculation of the
molecular mass you must add the weight (mass) of the water of crystallization.
Example: Prepare 500 ml of 0.1 M solution of K2Cr2O7.
Example: How many ml of a 1 M solution of AgNO3 must be added to 100 ml of a 1 M solution

of FeCl3 to precipitate all the chlorine as silver chloride?
Example: How many ml of 2 M NaOH solution are needed to precipitate all the copper present in
20 ml of 0.5 M CuSO4 solution?
Example: How many ml of 0.1 normal NaOH solution are needed to neutralize (neutralize) 20 ml
of 0.15 normal solution of H2SO4?
Example: Determine the normality of a solution that contains 1.96 grams of sulfuric acid in 200
ml of it.
30
Lab 5-ELECTROLYTIC DECOMPOSITION, REDOX REACTIONS
Molecules of electrolytes, acids, bases and salts during precipitation in water are broken down into
charged parts, into ions. This phenomenon is called electrolytic dissociation. Positively charged
ions are called cations, while negatively charged ones are called anions.
Electrolytic dissociation is a reversible process, therefore in electrolyte solutions, there is an

equilibrium between ions and undissociated molecules of dissolved electrolyte molecules is called
the dissociation rate.
Usually, the degree of dissociation is expressed as a percentage.

Depending on the degree of dissociation, electrolytes are divided into strong, medium and weak.
The degree of dissociation of strong electrolytes is greater than 30%; that of medium electrolytes
is 2-30% and that of weak electrolytes is below 2%.
As the solution is diluted, the rate of dissociation increases. Therefore, when comparing the
strength of electrolytes, solutions with the same normality should be taken. We can determine the
relative strength of electrolytes based on the electrical conductivity of their solutions and, based
on the chemical activity in some reactions.
The properties of aqueous solutions of acids and bases are determined by the ions into which they
dissociate. Acids are electrolytes, which release hydrogen cations in aqueous solutions. Bases are
electrolytes that release only hydroxyl anions in aqueous solutions
Such electrolytes are known, which release simultaneously hydrogen cations and hydroxyl anions
during dissociation. Such compounds are called amphoteric electrolytes. As an example of an
amphoteric electrolyte, we can mention aluminum hydroxide Al(OH)3 whose molecules dissociate
as an acid and as a base.
The degree of dissociation determines the possibility of the formation of acid salts and basic salts.
During the interaction of electrolyte solutions, reactions take place between the ions of the
dissolved substances (substances). The equations of these reactions can be presented both in
molecular form and in ionic form, for example:
Excluding from the equation of ions the symbols of ions that have not entered into chemical
interaction (Na+ and Cľ), we can write the equation in a simpler form:
During the interaction of acids and bases, H+ and OH ions combine to form water molecules. This
process is called neutralization. The formation of a gram-molecule of water from H+ and OH ions,
during the neutralization of strong acids with strong bases is accompanied by the release of 13.7
kilocalories of heat, which is called the heat of neutralization.
A solution containing an equal number of H and OH ions is called neutral. A solution in which H+
ions predominate is called acidic, while a solution in which OH ions predominate is called alkaline.
The acidity and alkalinity of the environment are determined by reagents that change their color;
31
depending on the relative concentrations of H and OH ions. These reagents are called indicators.
As an indicator, we use lakmevies, methyl orange, phenolphthalein, etc.
1) device to observe electrical conductivity according to fig. 58; 2) accumulator of 2-4 volts; 3)
ammeter of 3-5 amperes; 4) coal electrodes 2 pieces; 5) measuring cylinder with pupil 100 ml - 2
pieces; 6 glass jars; 9) bark cork, 10) plywood circle; 11) test tube holder; 12) rubber hoses; 13
wire, 14) sample.
Reagents and materials: 1) zinc (granular) 2) ferrous sulfate (divalent) FeSO4.7H2O.
Solutions: 1) hydrochloric acid HC1 (2 normal, 1 normal and 0.1 normal); 2) sulfuric acid H2SO4
(2 normal and 1 normal); 3) acetic acid CH3COOH (1 normal and 0.1 normal). 4) potassium
hydroxide KOH(2 normal); 5) sodium hydroxide NaOH (2 normal) 6) ammonium hydroxide
NH4OH (2 normal and 1 normal) 7) silver nitrate AgNO3 (0.1 normal) 8) sodium chloride NaCl
(2 normal) 9) potassium chloride CaCl2 (2 normal) 10) copper chloride CuCl2 (0.5 normal); 11)
ferric chloride FeCl3 (0.5 normal); 12) potassium chlorate KClO3 (1 normal); 13) ferrous sulfate
(bivalent) FeSO4 (0.5 normal); 14) ferric sulfate (trivalent) Fe2(SO4)3 (0.5 normal); 15) zinc
sulfate ZnSO4(0.5 normal) 16) sugar; 17) ethyl alcohol C2HsOH; 18) litmus; 19) methyl orange;
20) phenolphthalein (alcoholic solution)
Practical work
I. Electrical conductivity of the solution
Connect, in the circuit, an electrical pot and two electrodes (thick copper wires) located in a large
round plug. Immerse the electrodes in distilled water, with which the pot is filled, the pot will not
ignite. Immerse the electrodes alternately in the sugar and alcohol solutions also prepared with
distilled water. Again the pot will not turn on.
Do the same with aqueous solutions of HCI, NaOH and NaCl. Before each test, rinse the container
and the electrodes with distilled water: Always turn on the pot.
2. Electrical conductivity of solutions of some acids and alkalis
Take an accumulator (2-4 volts), an ammeter (3-5 amps) and 2 carbon electrodes (rods) placed in
a circle of plywood. Connect the apparatus according to 59. The carbon electrodes should be
dressed with rubber tubes, which completely cover the upper part of the rods. Pour 100 ml of 1
normal solution of hydrochloric acid, sulfuric acid and acetic acid into three glasses.
Immerse the electrodes in the beaker of hydrochloric acid so that the lower parts of the rubber
tubes are slightly submerged in the liquid. This is done so that in all the experiments that are done
there is always the same uncovered surface of the electrodes. Note the ammeter needle reading.
Then dip the electrodes alternately into the beakers containing sulfuric acid and acetic acid. Note
the ammeter readings.
32
During the transition from one solution to another, the electrodes must be rinsed with distilled
water before immersing them in the new solution. Compare the electrical conductivities of the
acids analyzed and conclude on their relative strength. This is how you test electrical conductivity
of normal sodium hydroxide and ammonium hydroxide solutions. Compare the dissociation rate
of these alkalis.
3. Comparison of the chemical activity of solutions
a) Pour 5 ml of 0.1 normal HCl solution into one test tube and pour the same amount of 0.1 normal
CH3COOH solution into another.
Pour an approximately equal piece of zinc into each test tube. Observe the evolution of hydrogen
and note in which of the test tubes the hydrogen is liberated more energetically. Explain this.
Pour some calcium chloride solution into two test tubes. Add 2 normal NaOH solutions to one test
tube and the same volume of 2 normal NH4OH solutions to the other (the NaOH and NH4OH
solutions must not contain carbonates). Note the phenomenon of precipitates in both test tubes.
Explain the cause of the different action of the bases obtained on calcium chloride.
4. Coloring of repellents (indicators).
a) Pour a little distilled water into three test tubes and add a few drops of solutions of the indicators
(indicators) to each of them: vitreous, methyl orange and phenolphthalein. Put their color in the
water in the neutral environment.
Add an acid solution to each test tube. Note the color change in acidic medium.
b) Do this by taking the solution of an alkali instead of the acid.
5. Heat production during neutralization
a) Take 50 ml each of 2 normal solutions of NaOH and HCl. Pour these solutions into 2 separate
beakers and measure the temperature of one of the solutions. Mix the acid with the alkali in one
beaker and carefully stir the liquid with the side of the thermometer. Note the rise in temperature.
Write the equation in molecular form and in ionic form.
How do you explain the equal rise in temperature in these two different experiments?
6. Reaction on chloride anion
a) Pour the diluted HCl solution into a test tube and add a few drops of AgNOz solution; Note the
separation of the precipitate. In this way, test the action of AgNO3 on the dissolution of NaCl,
CuCl2 and FeCl3 in separate test tubes. Write the equations of the reactions in molecular form and
in ionic form. Which abbreviated ionic equation can express all four of these reactions?
b) Mix the AgNO3 solution with the KCIO3 solution. Explain why the AgCl precipitate does not
form?
33
7. The difference between divalent and trivalent iron ions (ferrous and ferric).
Look carefully at the colors of the FeSO4 and Fe2(SO4)3 solutions. Mix the freshly prepared
FeSO4 solution with the NaOH solution in a test tube. In another test tube, mix the solution of
Fez(SO4)3 with the solution of the same alkali. Note the formation of precipitates and their color.
Write the equations of the reactions in molecular form and in ionic form.
8. Amphoteric electrolytes
a) Pour the ZnSO4 solution into a test tube and add a few drops of NaOH solution. Note the
formation of a white precipitate of Zn(OH)2. Write the reaction equation in molecular form and in
ionic form.
b) Shake the contents of the test tube of the above experiment and the precipitate and pour
approximately half of it into another test tube. In one of the test tubes, add the HCI solution, while
in the other, the NaOH solution (in excess). In both cases, dissolution of the precipitate will occur.
Write the equations of the reactions in molecular form and in ionic form.
Lab 6-CHEMICAL EQUILIBRIUM IN ELECTROLYTE SOLUTIONS
In weak electrolytes, the dissociation of molecules into ions is a reversible process. This means
that, in addition to the division of molecules into ions, the fusion of ions into molecules occurs
simultaneously.
When the speeds of these two opposite processes become equal, a state of equilibrium is reached,
where in the unit of time, as many molecules are divided into ions as are formed by the union of
ions.
The process of electrolytic dissociation, as a reversible process, is subject to the law of mass action;
for example, for an electrolyte AB at a given temperature we can write:
This expression shows that the equilibrium will be established when the ratio of the product of ion
concentrations against the concentration of undissociated molecules of the electrolyte is equal to a
constant value K. This value is called the dissociation constant of the electrolyte.
From the magnitude of the dissociation constant, one can judge the tendency of the electrolyte to
split into ions. The stronger the electrolyte, the greater will be the concentrations of ions (in the
numerator) and consequently, the greater will be the value of the dissociation constant.
The dissociation constant does not depend on the dilution of the electrolyte solution, so in many
cases, to determine the strength of the electrolyte, it is better to rely on the dissociation constant
than on the degree of dissociation.
34
It should be noted that the usual expression for dissociation constants can be fully applied only to
very dilute solutions. of weak electrolytes.
Strong electrolytes exhibit large deviations from the law of mass action. But the general direction
of the reaction derived from the law of the action of masses usually remains true (straight) even
for strong electrolytes. By changing the concentration of ions, we can shift the equilibrium of the
solution to this or that side. In some cases the displacement of the equilibrium can be distinguished
by the change in the color of the solution (if the color of the ions is different from the color of the
undissociated molecules).
The application of the law of mass action in saturated solutions gives us the opportunity to explain
the conditions under which the formation or dissolution of precipitates in electrolyte solutions
occurs. In a saturated solution there is a dynamic equilibrium between the solid substance, in the
solution, and the molecules of this same substance that are in the solution.
In the case of electrolyte substances, in addition to the balance shown above, another balance is
established in the solution between the molecules of the electrolyte and the ions formed by them.
Thus, for example in the saturated solution of CaCO3 there are these equilibria:
The dissociation constant of this sparingly soluble salt is expressed by this equation:
In the case of a saturated solution, the concentration of undissociated molecules is an invariant

value. It follows that the product of the ion concentrations in a saturated solution is also an invariant
value. The solubility product characterizes the solubility of a slightly soluble electrolyte at a given
temperature. Of two salts of the same type, the salt with the lowest solubility product has the lowest
solubility.
In a saturated solution by changing the concentrations of ions we can shift the equilibrium. The
latter causes the precipitation or dissolution of the electrolyte precipitate.
Precipitation is caused by increasing the concentration of one of the types of ions contained in the
saturated electrolyte solution.
Example: In the saturated solution of CaCO3, adding a concentrated solution of Na,CO3 increases
the concentration of CO23 ions, which will cause the displacement of the equilibrium in the
direction of the formation of new molecules of CaCO3. Given that the solution is saturated and
that the concentration of (dissolved) CaCO3 molecules in it, for a given temperature, has an
invariable (constant) value, then the formation of new molecules should cause the exit (or increase)
of the precipitate.
The dissolution of the precipitate is caused by the decrease in the ion concentration. This reduction
of ions can be done by throwing into the saturated solution in the presence of hesitate, the solution
of another electrolyte containing such that with the type of ion present in the saturated solution, it
forms molecules of a substance that dissociates very little.
35
Practical Work
Ring stand; 2) lamp; 3) measuring cylinder with 25 ml pupil; 4) porcelain bowls and cups; 5)
asbestos mesh; 6) test tube holder and 7) test tube).
Reagents and materials:
zinc (granules or slabs); 2) cobalt chloride CoCl2. 6H2O;3) cupric nitrate Cu(NO3)2. 6 H2O; 4)
sodium acetate CH3COONa;5) calcium oxalate CaC2O4; 6) calcium hydroxide Ca(OH)2; 7) ethyl
alcohol C2H2OH.
Solutions: hydrochloric acid HCI (concentrated and 2 normal); 2) acetic acid CH3COOH (2
normal and 0.1 normal); 3) potassium chloride KCI (saturated); 4) barium nitrate Ba(NO3)2
(saturated); 5 barium chloride BaCl2 (saturated); 6) potassium chlorate KClO3 (saturated); 7)
sodium chlorate NaClO3(saturated); 8) sodium acetate CH3COONa(2 normal); 9) methyl orange.
1. Color of molecules and ions
a) In a small porcelain cup, place some small crystals (crumbs) of cobalt chloride CoCl2. 6H2O
and heat until all water of crystallization is removed. Note the change in color of the salt (it turns
blue). After cooling, dissolve the salt remaining without water in a small amount of ethyl alcohol.
The color of the solution should again remain blue. Add water to the solution and notice the color
change from blue to rose (pink). The blue color belongs to undissociated CoCl2 molecules, while
the pink one belongs to cobalt ions (or more precisely to hydrated cobalt ions).
b) Dissolve some crystals of copper nitrate in a small amount of water; you will get a green colored
solution. Add some water. Note the color change of the solution from green to blue. Give the
explanation.
2. Shifting the balance of ions
a) Dissolve a few small crystals of cobalt chloride in as little water as possible. Note the color of
the solution. Add concentrated hydrochloric acid to the solution until it changes color (to blue).
Write the equation for the dissociation of CoCl2 into ions. Explain the color change based on the
law of mass action.
b) Put 5 ml of 0.1 normal solutions of acetic acid in a test tube, while in another test tube 5 ml of
water. Add 2-3 drops of methyl orange to both test tubes. Leaving the test tube with water aside
for comparison, drop a pinch of sodium acetate into the acetic acid solution. Note the color change
of the methyl rose from pink to yellow. How did the concentration of hydrogen ions in this solution
change after you added CH3COONa? Give an explanation based on the law of mass action.
3. Reciprocal action of the salt of a weak acid with a strong acid.
Pour 5 ml of 2 normal solutions of hydrochloric acid into two test tubes and pour an equal piece
of zinc into each of them. When the release of hydrogen is observed in the two test tubes, then in
36
one of them pour 5 ml of 2 normal solution of CH3COONa, while in the other pour 5 ml of water.
Note the apparent slowing down of the reaction (of H2 release) in the first test tube. Write the
equations of the reactions in molecular form and in ionic form.
Applying the law of the action of masses, explain why adding a salt of a weak acid to the solution
of a strong acid decreases the reactive power of the latter.
4. Precipitation of the electrolyte by increasing the human concentration of his descendants.
a) Put the saturated potassium chlorate solution into two dry test tubes. In one add a little saturated
solution of KCl, while in the other add a little saturated solution of NaClO3. Mix the contents of
the test tubes. Note the formation of precipitate in both test tubes. Express the solubility product
equation of potassium chlorate. Explain the formation of the precipitate of this salt after the
addition of KCl or NaClO3 solution.
b) Pour saturated solution of BaCl2 into one test tube, while pour saturated solution of Ba(NO3)2
into another. In the first test, tube add a little concentrated hydrochloric acid, while in the second
add a little concentrated nitric acid. In both cases, notice the formation of a precipitate. Based on
the solubility products of salts, explain the turbidity of solutions.
5. Dissolving the precipitate of an electrolyte
a) Put some slaked lime, some water in a test tube and then mix them. Add dilute hydrochloric
acid to the saturated solution obtained in this way, but which also contains undissolved lime. Note
the complete dissolution of the lime. Write the equation for the solubility product of Ca(OH)2 and
the equation for the reaction between hydrochloric acid and calcium hydroxide in ionic form.
Explain the solubility of Ca(OH)2 in hydrochloric acid.
b) Put some dry calcium oxalate CaC2O4 into two test tubes. Add hydrochloric acid to one of the
test tubes, and acetic acid to the other. Note the dissolution of CaC2O4 only in the first test tube
and the lack of reaction in the second test tube. Explain the different action of these two acids on
calcium oxalate by considering the degree of dissociation of hydrochloric, oxalic and acetic acids.
Lab 7-HYDROLYSIS OF SALTS AND COLLIGATIVE PROPERTIES
The phenomenon of hydrolysis is related to the ability of water to dissociate (even in a very small
amount) into ions based on this equation: OH= H + OH
The concentration of hydrogen ions and hydroxyl ions in chemically pure water is equal, therefore
the water has a neutral reaction.
During the dissolution of many salts in water, their ions obtained during dissociation enter into
mutual action with water ions. In this case, the connection of one of the ions (H+ or OH') with the
salt ions can occur, and in this so that the ionic balance of the water is disturbed and the solution
receives an alkaline or acid reaction.
The process of the interaction of the ions of a dissolved salt with the ions of water is called salt
hydrolysis.
37
Hydrolysis of salts consists of two reciprocal processes:
1. From the dissociation of water molecules into H' and OH' ions, and
2. from the interaction of the formed H' and OE' ions with the salt ions present in the solution.
So e.g. The hydrolysis of sodium acetate can be represented by this scheme:
CH3COONa = CH3COO- +Na+
H2O= H+ +OH
From the scheme shown above, it can be seen that the H' ions of water bind to the CH3COO'
ions forming acetic acid molecules that dissociate slightly, which causes the amplification of
water dissociation and the further binding of H+ ions.
As a result, the concentration of OH ions increases in the solution, while the concentration of H'+
ions decreases and the solution reaction becomes alkaline. Hydrolysis reactions can be expressed
by equations
common chemicals, for example:
CH3COONa+H2O CH3COOH+NaOH or by ionic equations for example:
CH3COO+H2O CH3COOH+OH
The solutions of most salts, thanks to hydrolysis, have an acid or alkaline reaction. Only in cases
where the salt subjected to hydrolysis is formed by the mutual action of a strong acid with a strong
base (with almost equal strengths), then the salt solution will be neutral, e.g. NaCl, KNO3).
Hydrolysis in these cases will not occur.
Hydrolysis is a reversible process.
The degree of hydrolysis is called the ratio of the number of hydrolyzed salt molecules to the total
number of salt molecules present in the solution. The rate of hydrolysis increases with increasing
temperature and dilution of the solution.
The hydrolyzed part of the salt, in many cases, is very small, so e.g. at 25°C in 0.1 normal
solutions the rate of hydrolysis is:
for sodium acetate - 0.007%
for potassium cyanide-1.2%
for sodium carbonate -2.9%
Salts formed by the mutual action of weak acids and weak bases are more hydrolyzed. In this case,
the hydrolysis reaction can practically go to the end.
38
Hydrolysis can also be taken as a decomposition process, by which the salt with water forms the
acid and the base, ie. as the opposite reaction of neutralization.
Sometimes, during hydrolysis, instead of acids and bases, acidic or basic salts are formed. Acid
salts are produced during the hydrolysis of salts of (weak or medium) dibasic and polybasic acids,
e.g.
Na2S+H2O= NaHS +NaOH
Basic salts can be formed during the hydrolysis of divalent and polyvalent metal salts for
example:
ZnOHCl+HCl
Practical Work
Apparatus and containers: 1) measuring cylinder with 10 ml pupil; 2) funnel; 3) glass birch; 4)
test tube holders; 5) lamps; 6) test tubes.
Reagents and materials: 1) magnesium (powder); 2) zinc (grain); 3) litmus paper 4) filter paper.
Solutions 1) hydrochloric acid HC1 (2 normal); 2) sodium chloride NaCl (2 normal); 3) ferric
chloride FeCl3 (2 normal); 4) antimony chloride SbCl, (O.5 normal); 5) aluminum salt for example
AlCl3 (O.5 normal); 6) sodium carbonate Na,CO3 (2 normal); 7) sodium acetate CH3COONa (2
normal and 0.5 normal); 8) sodium sulfide Na2S (2 normal); 9) potassium nitrate KNO2 (2normal);
10) sodium sulfite Na2SO3(2 normal); 11) phenolphthalein (alcoholic).
1. Salt dissolution reaction during hydrolysis
a) Pour a little solution of sodium sulphide or potassium nitrite into a test tube and test its action
on litmus. For this, put a drop of solution on the tracing paper with a glass rod. Write the equation
for the hydrolysis reaction of the resulting salt.
b) Write the equations for the hydrolysis reactions of copper sulfate and sodium sulfite. Infer how
their digestions must act on the covetous. Test the accuracy of your conclusion by experimenting
with solutions of these salts on tracer paper.
c) What reaction will the beggar show when immersed in table salt solution? Test the accuracy of
your conclusion by means of an experiment.
d)Pour some solution of ferric chloride of trivalent iron into a test tube and test its action on tracer
paper. Write the equation for the hydrolysis reaction of FeCl3. Add some powdered magnesium
to the ferric chloride solution. Note the release of hydrogen. Give an explanation.
2. The influence of temperature on hydrolysis
Mix in a test tube 5 ml of solutions of ferric chloride and sodium acetate with equal concentrations
(1 normal). Heat the liquid until it boils. Note the separation of a red-brown precipitate of basic
39
ferric acetate. Write the equations for the reactions between FeCl3 and CH3COONa to form ferric
acetate and between ferric acetate and water to form Fe(OH)2(CH3COO).
3. The influence of dilution of the solution on hydrolysis
Pour one ml of antimony chloride solution into the test tube and dilute with water. Note the
formation of the basic salt precipitate.
Write the equation assuming that the reaction proceeds to the formation of the basic salt
Sb(OH)2Cl, which then loses water and turns into antimony chloride (SbOCl). Save the solution
together with the obtained precipitate for the next experiment.
4. Susceptibility of hydrolysis
a) Add to the solution of antimony chloride together with the precipitate of the basic hydrochloric
acid salt until all the precipitate is dissolved. Then dilute the solution again with water. Explain
the observed changes.
b) Put some 0.5 normal sodium acetate solution in a test tube and add 2-3 drops of phentolphthalein
solution. Heat the liquid until it boils. Note the appearance of pink color in the digest. During the
cooling of the solution the color disappears again. Explain the observed changes.
5. Complete hydrolysis
c) Pour the solution of aluminum salt and the solution of Na2CO3 into a test tube. Note the
formation of a white amorphous precipitate and the formation of bubbles of CO2. Heat the tube,
filter the precipitate and rinse it over the filter with hot water to remove excess Na2CO3.
Prove that the formed precipitate is not carbonate salt, but aluminum hydroxide. For this, divide
the precipitate into two parts; act on one of them with dilute hydrochloric acid, while on the other
with sodium hydroxide. In both cases, dissolution of the precipitate occurs. Focus attention on the
fact that no gas is released during the dissolution of the precipitate in HCl.
Write the equation for the hydrolysis reaction that occurs between aqueous solutions of aluminum
salt and Na2CO3.
Lab 8-HYDROGEN, HYDROGEN PEROXIDE. OXYGEN.
Hydrogen
The hydrogen atom consists of a nucleus, which has a positive charge (proton) and an electron.
When combining hydrogen with atoms of other elements (of metalloids), the hydrogen atoms give
them the electron and become positively charged. Therefore, the valence of hydrogen is +1. In
some cases (in the case of reactions with the most active metals), hydrogen atoms can attract
electrons by becoming negatively charged. These compounds of hydrogen with metals are called
hydrides.
40
Under normal conditions, hydrogen is a colorless, odorless gas. It is the lightest of all gases, it is
14.5 times lighter than air (1 liter of hydrogen under normal conditions weighs about 0.09 grams).
Its melting point is -259°C, while its boiling point is -253 °C. The solubility of hydrogen in water
is very small (2% by volume).
The hydrogen molecule consists of two atoms strongly bonded to each other, therefore, at the usual
temperature, it is slightly active from the chemical point of view and binds only to fluorine and
chlorine (the latter requires strong illumination).
As the temperature increases, the bond between the atoms in the hydrogen molecule weakens and
its activity increases. Hydrogen combines more easily with metalloids. Hydrogen forms water by
burning in oxygen or air. The mixture of two volumes of hydrogen with one volume of oxygen has
maximum explosive power and is called explosive gas.
When heated, hydrogen readily combines with many substances, exhibiting strong reducing
properties. The newly born hydrogen is more active because it is in the atomic state.
In the laboratory, hydrogen is prepared by reacting zinc with hydrochloric acid or dilute sulfuric
acid. In addition, hydrogen can be prepared by the interaction of some metals with water, with
alkali solutions, or by electrolysis of water.
Appliances and utensils:
1) gasometer with oxygen
2) Kip's apparatus with filling for cooking hydrogen;
3) apparatus for cooking hydrogen (container with 200 ml pupil, test tube with a hole at the
bottom, glass tubes, rubber tubes, clamps, two test tubes;
4) tripod with clips;
5) lamp;
6) test tubes with corks and tubes with bent ends
7) glass cylinder;
9) student glasses 50-100ml;
10) glass plates; (3 pieces)
11). test tube holders,
12) test tubes.
41
1) Zinc (grain); 2) aluminium (powder); 3) cupric oxide CuO. Solutions: 1) sulfuric acid H2SO4
(1:5); 2) sodium hydroxide NaOH (10%); 3) potassium permanganate KMnO4 (0.1 normal).
Practical work
Note: Hydrogen produced by an apparatus should never be ignited without making sure it is
completely clean, otherwise we will have very dangerous explosions.
1). Preparation of hydrogen by the action of the metal
With acid extended and after fixing the test tube vertically in the tripod clamp, observe the
formation of gas. You must ensure that the hydrogen coming out of the apparatus is not mixed
with air. For this, you should place a test tube (fig. 52) on the extended pipe, keeping it in position
for about half a minute as in fig. 52. Then remove the inverted test tube and bring it closer to the
flame of the lamp. If there is pure hydrogen in the test tube, it will ignite quietly (a faint noise is
heard during ignition) and with a faint blue flame. If there is air in the test tube along with the
hydrogen, then a small crack occurs accompanied by a sharp sound. In this case, the gas purity test
must be repeated. After you are satisfied that pure hydrogen is coming out of the test tube, it can
be ignited. Hold a dry beaker over the hydrogen flame. Note the small water droplets covering the
sides of the glass
2. Preparation of hydrogen by the action of metal with alkali
Set up an apparatus consisting of a test tube with a cork, through which a glass tube with an
elongated tip passes. Place a few grains of zinc in the test tube and fill 1/3 of it with dilute sulfuric
acid. After you have properly placed the cap with the pipe
In a test tube, pour caustic soda solution then add some aluminum powder (or sawdust). Observe
the formation of gas. Close the test tube with a stopper with an elongated tube and after making
sure that the air has completely left the test tube, turn on the gas.
During the interaction of aluminium with NaOH solution, the reaction takes place in two stages:
2A1(OH)3+2NaOH=2NaAlO2+4H2O.
The general equation for this reaction is:
2Al+2H2O+2NaOH=2NaAlO2+3H2
3. Pouring hydrogen from one container to another
Fill a cylinder (or a test tube) with hydrogen from Kip's apparatus. Slowly pour the hydrogen in
the cylinder into another cylinder, upside down with the nozzle down. By bringing the flame of
the gas lamp nearer to the two inverted cylinders, you will see that the second cylinder will either
flame or hear a slight crackling, while in the first cylinder (which now has no more hydrogen) this
42
nothing will happen. So, you will be convinced that the hydrogen has passed from the first cylinder
to the second from the bottom up.
4. Combustion of explosive gas.
Fill a small cylinder (or a test tube) full of water, cover it with a glass plate and invert it into a
crystallizer (bath) with water. Then fill the cylinder up to 1/3 with oxygen (from the gasometer)
and the remaining 2/3 with hydrogen (from Kip's apparatus). Take the cylinder out of the
crystallizer by holding it end up and covering its mouth down with a glass plate. Wrap the cylinder
with a towel and, after removing the glass plate, bring it close to the flame of the lamp. A strong
explosion occurs from the mixture's combustion.
5. The reducing properties of hydrogen
Fix a dry test tube with a small amount of cupric oxide to the tripod clamp at an angle (with the
end raised).
Set up an apparatus for cooking hydrogen (see left part of figure 53), consisting of a container
(bottle) of dilute sulfuric acid, a test tube with a hole in the bottom filled with zinc grains, and a
funnel with clip that serves to remove the gas from the test tube. In this apparatus, the test tube is
inserted into the stopper that closes the container (bottle).
After immersing the zinc test tube in sulfuric acid and removing the cap, you must first test the
purity of the hydrogen coming out of the apparatus.
When the hydrogen comes out clear, let it pass into the tube containing the cupric oxide. First,
keep the sample at room temperature and then heat it. Note the changes that occur in the cupric
oxide as well as the formation of water droplets on the faces. Newborn hydrogen. After coloring
the diluted H2SO4 solution with a few drops of KMnO4 solution, divide it into two test tubes.
Drop a piece into one of them zinc which does not contain arsenic, while in the other send hydrogen
from Kipp's apparatus. Compare the rate of color change of the solution in both test tubes, explain
the difference in the rate of loss of color of the solution. The reaction of reduction of potassium
permanganate by means of hydrogen takes place on the basis of this equation:
KMnO4+10H+3H2SKMnO4+10H+3H2SO4=2MnSO4+K2SO4+8H2O
=2MnSO4+K2SO4+8H2O
Hydrogen Peroxide
Hydrogen peroxide, H2O2, is a colorless, syrupy liquid with a specific gravity of 1.46. It is an
unstable compound and decomposes even in the cold. In dilute aqueous solutions, it is more stable,
but it nevertheless decomposes quickly in the presence of some manganese dioxide or alkali
catalysts, etc. The aqueous solution of hydrogen peroxide has the properties of a weak acid. By
reacting with bases, it forms salts called peroxides, such as sodium barium peroxide, etc. (Na2O2,
BaO2, etc.).
43
Hydrogen peroxide is a strong oxidizer and its use for bleaching silk, furs, rejuvenating paintings,
in medicine (for gargles for rinsing wounds, etc.) is based on this property. In some reactions,
hydrogen peroxide can also play the role of reducing substance.
When hydrogen peroxide behaves as an oxidizing substance it decomposes releasing atomic

oxygen. When it behaves as a reducing substance, it decomposes releasing atomic hydrogen and
oxygen molecules.
Hydrogen peroxide is usually produced by the action of diluting H2SO4 on barium peroxide BaO2
or sodium peroxide Na2O2.
Hydrogen peroxide can be detected in a solution by the following reactions:
a) During the interaction of H2O2 with K2Cr2O7 in an acidic environment, the unstable chromium
peroxide CrOs with a blue color is prepared, which dissolves better in ether than in water.
b) During the interaction of H2O2 with KI in an acidic environment (eg hydrochloric acid) free
iodine is released, which will give the solution a yellow or brown color. In this case, this reaction
takes place:
The presence of iodine can also be indicated by means of starch cough, which acquires a blue color
from iodine. The last reaction is more sensitive than the first, that is, it allows to detect of smaller
amounts of hydrogen peroxide.
Appliances and utensils:
1) technical-chemical scale with weight box;
2) measuring cylinder with 25 ml pupil;
3) funnel
4) test tube holders;
5) glass beaker, 6) test tube.
1) sodium peroxide Na2O2;
2) barium peroxide BaO2;
3) manganese dioxide MnO2;
4) ether;
5) starchy cough;
6) ice;
44
7) dyed wool;
8) litmus paper;
9) filter paper;
10) birch wood.
Solutions:1) hydrogen peroxide H2O2 (30% and 3%); 2) sulfuric acid H2SO4 (2 normal); 3)
aqueous solution of ammonia NH4OH (2 normal); 4) barium hydroxide Ba(OH)2 (saturated); 5)
lead nitrate Pb(NO3)2; (0.5 normal); 6) silver nitrate AgNO3 (0.1 normal); 7) potassium iodide KI
(0.1 normal); 8 potassium dichromate K2Cr2O7 (0.5 normal); 9) aqueous solution of hydrogen
sulfide gas H2S.
Practical work
1. Reaction for the detection of hydrogen peroxide
a) Pour water up to 1/3 of its volume into a test tube and then add 2-3 drops of potassium
dichromate solution and the same number of diluted H2SO4 drops also add 0.5 ml ether and a little
3% H2O2 solution. Mix the liquids by shaking the test tube. Note the blue coloration of the ether
layer.
b) In a test tube containing one ml of 3% H2O2 solution, add 1-2 drops of KI solution and a few
drops of diluted H2SO4. Also, add 1-2 drops ml of starch cough syrup to the test tube. Note the
blue color form.
Preparation of hydrogen peroxide
a) Pour about 5 ml of distilled water into a test tube and, mixing it with a glass rod, add 3-4 crumbs
of sodium peroxide. Cool the test tube in water and then add drops of diluted sulfuric acid until an
acid reaction is achieved. weak (litmus test). Divide the obtained solution into 2 parts.
One part test the existence of H2O2 by the dissolving action of K2Cr2O7 in the presence of ether,
while in the other part prove the existence of H2O2 by the dissolving action of KI in the presence
of starch .
Write the reaction equation for the formation (cooking) of H2O2.
b) In a well-chilled test tube on ice, take about 1.0 grams of powdered barium peroxide and add
little by little 5 ml of dilute sulfuric acid, mixing it with a glass rod. Filter the cloudy liquid from
the BaSO4 precipitate. Test for the presence of H2O2 in the filters.
Write the reaction equation for the formation (cooking) of H2O2.
3. Catalytic decomposition of hydrogen peroxide
Pour 1-2 ml of 3% H2O2 solution and then some manganese dioxide into a test tube. Test the
released gas with a slowly burning wooden stick. Write the reaction equation.
45
4. Oxidizing properties of hydrogen peroxide
To a test tube containing lead nitrate solution add hydrogen sulphide solution. Note the formation
of a black precipitate of lead sulphide. Write the reaction equation. Filter the precipitate, rinse with
water, then pour over the filter with 3% H2O2 solution until it turns white. Write the equation of
the reaction taking into account that during the interaction with H2O2 lead sulfide is converted to
lead sulfate.
5. Reducing properties of hydrogen peroxide
Pour 2-3 ml of silver nitrate solution into a test tube and add ammonium hydroxide solution drop
by drop (do not take in excess) until the formed turbidity is dissolved. Add 3% H2O2 solution to
the produced solution. Note the formation of a dark precipitate (metallic silver) and the evolution
of gas (prove it by means of the burning birch). Explain the observed changes. Write the equations
of the reactions.
6. Bleaching with hydrogen peroxide
Take some black wool and process it to remove the fat with a dilute alkaline solution and then
immerse it in a test tube containing 3% H2O2 solution. After a few hours notice the color change
of the wool.
7. Preparation of barium peroxide
Add 30% solution of hydrogen peroxide drop by drop to the saturated solution of Ba (OH)2. A
precipitate of brilliant, plate-shaped crystals with the composition BaO2.8H2O is formed.
Exercises and problems
1. Give examples of reactions in which H2O2 is reduced.
2. In which of the reactions below is hydrogen peroxide oxidizing and in which reducing:
Cl2+H2O2=2HC1+O2
MnO+H2O2=MnO2+H2O
3. How many litres of oxygen measured under normal conditions will be released from the
decomposition of 100 grams of a 4% solution of H2O2?
Oxygen
Oxygen is a typical element of group VI of the periodic system. Oxygen atoms have 6 electrons
in their outer shell. therefore, they easily receive two electrons, displaying negative valence 2 in
all compounds, except for OF2, where oxygen presents 2 positive valences.
Oxygen is a colorless and odorless gas slightly heavier than air. It boils at -183°C. It is soluble in
water (5/100 of the volume at O°C).
46
Oxygen is a chemically active element. It combines directly with almost all elements except the
inert gases, fluorine, chlorine, bromine, gold iodide, and platinum.
Compounds of elements with oxygen are called oxides.
Oxides are divided into basic, acidic and amphoteric. Basic oxides are formed only by metals; with
water these give bases. Acidic oxides with water give acids. Acidic oxides are mainly metalloid
oxides, although some low-valent metal oxides are also acidic. Amphoteric oxides also include
metal oxides, whose hydrates can behave as both acids and bases.
The production of oxygen under laboratory conditions is based on the breakdown of stable
oxygenated compounds; among these substances are: Bertole's salt, potassium permanganate,
sodium peroxide, mercury oxide, etc. During heating, these substances decompose releasing
oxygen.
Decomposition of Bertollet's salt is a reaction most often used for laboratory cooking of oxygen.
This reaction is extremely accelerated and takes place at a temperature lower than 300°C in the
presence of some oxides (for example MnO2, other Fe2O3), which themselves in this case do not
change chemically.
Substances that change the speed of the reaction, but that retain the same composition and quantity
after the reaction as they were before the reaction, are called catalysts.
In addition to oxygen, whose molecules are diatomic, a gas consisting of molecules, triatomic O3,
called ozone, has also been known. Ozone is a blue gas. Its melting point is - 251C. It boils at -
112°C. It dissolves in water better than oxygen (59: 100 by volume at O℃).
At ordinary temperature, ozone is usually stable, with heating it is easily converted into oxygen. It
readily releases an oxygen atom and is therefore a very strong oxidant.
Ozone is produced by the action of quiet electrical discharges on oxygen in devices called
ozonators, as well as by the action of concentrated sulfuric acid on barium peroxide.
Apparatus and containers: 1) technical-chemical scale with weight box; 2) gasometer filled with
oxygen; 3) tripod with clips; 4) lamps; 5) glass jars or cylinders with stoppers or glass plates and
pieces; 6) glass crystallizer; 7) porcelain bowl; 8) corks with pipes for gas extraction; 9) pliers for
the cones; 10) iron spoon for burning - 2 pieces; 1 holder with test tubes.
1) sulfur (cane); 2 magnesium (bar); 3) charcoal (pieces); 4) red phosphorus; 5) iron (wire); 6)
manganese dioxide MnO2; 7) barium peroxide BaO2); 8) potassium chlorate KClO3; 9) potassium
nitrate KNO3; 10) litmus paper (litmus); 11) filter paper; 12) birch wood; 13) starch cough (starch);
14) table salt; 1%) snow or ice, 16) steel wire.
Solutions: 1) Sulfuric acid H2SO4 (concentrated) 2) potassium iodide KI.
Practical work
47
1. Preparation oxygen
For the preparation of oxygen in the laboratory, in most cases, Bertole's salt (potassium chlorate)
is used, which is decomposed by heating according to this equation:
This reaction is quite accelerated and takes place at low temperatures in the presence of manganese
dioxide, which plays the role of a catalyst.
Bertole's salt should be used with care because having a very small mixture of burning substances
(paper, coal, etc.) during rubbing or heating can give strong cracks. Also taking into account that
manganese dioxide sometimes becomes impure (contaminated) by organic substances, for their
removal MnO2 is carefully crushed. For experiments take finely ground potassium chlorate and
powdered manganese dioxide.
Pour about 0.3 grams of KCIO3 into a dry and clean test tube and fix it in the clamp of the stand.
Heat the end of the test tube, first slightly and carefully and then more strongly. When the salt has
melted and the gas has begun to come out, then you should test the gas by carefully inserting a
slowly burning wooden stick into the mouth of the test tube.
Pour about 0.3 grams of KClO3 into another clean and dry test tube, fix the test tube on the stand
and melt the salt at the lowest possible temperature. Remove the lamp and immediately pour into
the test tube some MnO2 previously prepared in powder form and well crushed. Insert the slowly
burning birch bark into the test tube without touching the salt.
Look carefully at the difference in the rate of oxygen release in these two experiments.
2. Oxygen collection
Weigh on the technical-chemical balance 3 grams of KCIO3 and 3 grams of MnO2 in the form of
crushed and cooled powder. Mix these in a porcelain bowl with a glass rod and then pour them
into a dry test tube. Weigh the sample together with the mixture (weight a). Lift the device as
shown in fig.49. First, fill the cylinder designated for gas collection with water, then close it with
a glass plate or a cork, drop it with the mouth down into the tub half filled with water and open the
mouth of the cylinder under water.
Remove the end of the gas-carrying tube from the water and begin by heating the mixture in the
test tube. First heat the test tube carefully along the entire length of the slide and then more strongly
in the place where the mixture is located. You must be careful not to melt the glass. By bringing
the birch close to the hole of the pipeline, you should make sure that oxygen is being released.
After that, bring the end of the pipe under the cylinder filled with water. Collect the oxygen in the
cylinder leaving some water. Take the pipeline out of the water and only then stop the heating
(why?). Close the container under the water with a glass or metal plate, take it out of the water and
put it on the table.
This is how you collect oxygen in three cylinders (or other containers). Heat the test tube with the
mixture until the KCIO3 is completely decomposed. After the experiment is finished, remove the
gas removal tube from the water and then remove the lamp.
48
If the oxygen is not enough to fill 4 containers, then fill the container that remains unfilled from
the gasometer. Save the oxygen-filled vessels for experiment 3.
After cooling, weigh the test tube containing the mixture of KCl and MnO2 (weight b). The change
(a-b) will give the weight of oxygen liberated. Calculate the theoretical production of oxygen
coming out of 5 grams of KCIO3 (weight c), Determine the production of oxygen as a percentage
of the theoretical production, based on the formula:
3. Burns with oxygen
For these experiments, use vessels filled with oxygen
a) Put a small piece of sulfur in an iron spoon and light it with the flame of the lamp, then put it
inside the vessel containing oxygen, lowering the spoon gradually (fig.50).
You should focus your attention on the difference between burning sulfur in air and in oxygen.
After burning, close the container and shake it well so that the sulfur-burning products dissolve in
the water.
b) Do such an experiment by taking some red phosphorus instead of sulphur.
c) Into the container containing oxygen, insert a previously lit magnesium strip, holding it with
iron tongs (you should not look at the lit magnesium for a long time, because this is very harmful
to the eyes). After burning, shake the contents. of the container (magnesium oxide with water).
d) Attach a thin steel wire to a wooden stick, at the end of which attach a small piece of coal. Light
the charcoal in the flame of the lamp and then put it in the container containing the oxygen. Iron
burns throwing sparks in all directions. Test with red and blue litmus paper (litmus) the solutions
of the oxides formed as a result of the combustion of the substances taken.
Write the equations of the combustion reactions of the substances obtained and the equations of
the reactions of coupling with water, of the oxides produced, of sulphur, of phosphorus and of
magnesium.
4.Burning in molten saltpeter
Take a dry test tube and fill it up to 1/3 of the height with potassium nitrate. Fix the test tube on
the tripod vertically above the metal base and heat until the salt melts. When bubbles of gas
(oxygen) start to emerge from the molten mass, light a piece of coal on the lamp, holding it with a
pair of pliers, and pour it into the test tube (fig.51).
Stop the heating. Coal burns with leaping vigor; sometimes it jumps out of the test tube (be
careful!).
When the charcoal has burned, drop a piece of sulfur into the test tube. Sulfur burns more rapidly
and in this case, so much heat is developed that the glass softens and the test tube changes shape.
5. Formation of ozone
49
Put some powdered barium peroxide in one test tube and put about 2 ml of concentrated sulfuric
acid in another test tube. Cool both test tubes by immersing them in a container of cold water (or
better in a cold mixture of ice and salt). Pour the sulfuric acid into the test tube containing the
barium peroxide and mix it with the glass rod while simultaneously cooling the test tube. The
reaction takes place according to this equation:
3BaO2+3H2SO4=3BaSO4+3H2O+O3
Ozone can be detected by smell (the smell should be taken carefully), by the blue coloration of red
litmus moistened with KI solution, or by the filter paper dish moistened with KI solution and
coughed up. starch (starch). During the action of ozone on KI, the following reaction takes place:
2KI+O3+H2O=2KOH+I2+O2
The litmus paper (litmus) turns blue from the alkali formed, while the starch powder turns blue
from the iodine.
Lab 9-HALOGENS
Chlorine and hydrochloride gas

The chlorine atom has 7 electrons in the outer shell, so it easily withdraws an electron, becoming
a monovalent negative ion, which characterizes it as a metalloid. The negative valence of chlorine
is therefore -1.
Chlorine atoms not only receive electrons, but under certain conditions, they can also give up to 7
electrons. Therefore, the maximum positive valence of chlorine is +7.
Giving electrons from chlorine is much more difficult than withdrawing them, so the substances
that are formed in this case (compounds of chlorine with oxygen) are less stable than chlorides in
which chlorine is negatively charged.
Free chlorine under normal conditions is a green to yellow gas and approximately 2.5 times heavier
than air (1 liter of chlorine under normal conditions weighs 3.21 grams). It dissolves quite well in
water. At ordinary temperature, 1 volume of water dissolves about 2 volumes of chlorine. This
solution is called chlorine water.
Chlorine is one of the most energetic elements. It enters into the reaction very easily and connects
directly with almost all elements, with the exception of oxygen, nitrogen and chromium. The
compounds of these elements with chlorine are obtained only indirectly (indirectly). Especially
chlorine acts energetically with metals. Thus, e.g. molten sodium metal burns in chlorine with a
dazzling light, in which case sodium chloride is formed.
Copper, iron, tin and other metals, preheated (before), also burn in chlorine to form the
corresponding salts .Moist chlorine and its aqueous solution - chlorine water - decolorize most
50
organic coloring substances. This is explained by the fact that chlorine partially reacts with water
to form hypochlorous acid: which oxidizes the coloring substances and thus decomposes them.
Table salt NaCl is used as the starting substance for chlorine production. All chlorine production
methods are based on the oxidation of the chloride ion to a neutral atom. In industry, this oxidation
is done by means of electrolysis, while in the laboratory it is done by means of different oxidizing
substances:
KMnO4, K2Cr2O7, PbO2, MnO2, etc. 2Cr2O7
One of the most important compounds of chlorine, which has wide industrial use, is hydrogen
chloride (hydrochloric gas). This can be produced by directly combining chlorine with hydrogen.
In the laboratory, hydrochloric acid is prepared by the action of concentrated sulfuric acid on table
salt. This is a colorless, strong-smelling (smelling) gas that emits smoke into the air (mist-forming).
Hydrogen chloride dissolves well in water. One volume of water under normal conditions
dissolves up to 525 volumes of hydrogen chloride gas. This dissolution of carbon dioxide in water
is called hydrochloric acid.
Apparatus and containers: 1) chlorine preparation apparatus (distillation pot, separating funnel,
two washing or drying containers); 2) Kip's apparatus, filled for cooking hydrogen; 3) iron plates,
4) iron pliers, 5 knives; c) cylinders with caps 5 pieces; 7) stands with clips and rings; 8) test tube
holders; 9) pipelines with stoppers; 10) thermometers; 11) glass beaker for cooling mixture.
Reagents and materials: 1) manganese dioxide MnO2; 2) potassium dichromate K2Cr2O7; 3)

potassium permanganate KMnO4; 4) sodium chloride NaCl; 5) copper (thin wire of electrical
conductors; 6) iron powder; 7) antimony (powder) 8) metallic sodium; 9) turpentine; 10) litmus
paper; 11) asbestos; 12) iron plate; 13) filter paper; 14) cotton; 15) ice, 16) sand.
Solutions: 1) hydrochloric acid HCl (concentrated); 2) sulfuric acid H2SO4 (concentrated and 2
normal); 3) sodium chloride NaCl; 4) potassium permanganate KMnO4 (concentrated); 5) NaOH
sodium hydroxide; 6) silver nitrate AgNO3; 7) fuchsia; 8) indigo; 9) litmus; 10) writing ink.
Practical work
Note: Do all work with chlorine and hydrochloric acid in a fume hood. Glass containers that can
be filled with chlorine, for various burns, are covered with a thin layer of sand.
a) Pour some manganese dioxide into a test tube and add about 1ml of concentrated hydrochloric
acid. Lightly heat the sample. Note the release of chlorine, which is distinguished by color and
odor. To distinguish the color of the gas, place a sheet of white paper behind the test tube. Be
careful when sniffing (do not take deep breaths). Write the reaction equation.
b) Put 2-3 potassium dichromate crystals in a test tube and add 1-2 ml of concentrated hydrochloric
acid. Then heat the test tube. Note the release of chlorine. Write the reaction equation.
c) Put some KMnO4 crystals in a test tube and add some concentrated hydrochloric acid. Note the
release of chlorine, which in this case occurs even without heating. Write the reaction equation.
51
d) Build an apparatus for cooking chlorine according to figure 60. Pour concentrated hydrochloric
acid into the still, while the separating funnel fill with concentrated solution of KMnO4. Pour
distilled water into the first washing container (to clean the chlorine from the HCI mixture), while
into the second drying container pour concentrated H2SO4 (to dry the chlorine). Loosely open the
funnel and drop the KMnO4 solution onto the hydrochloric acid. Collect the chlorine that is
released in a small beaker (or jar). Distinguish the filling of the container by the color of the gas
collected in it. Fill some glass containers (jars) with chlorine and cover them with watch glass or
glass plates. Save the jars filled with chlorine for future experiments.
2. Burning of metals in chlorine
a) Heat a bunch of copper wires and put them all at once in a container (jar) filled with chlorine.
Observe the burning of copper in chlorine. Write the reaction equation. After cooling the jar
(container), pour some water into it and shake. Note the staining of the digest. To better distinguish
the presence of Cu2+ ions, which were obtained from combustion, pour 3-5 ml of NH4OH.
b) In the corner of an iron plate, heat some iron powder until it becomes incandescent and then
shake it little by little in a container (jar) filled with chlorine. Observe the burning of iron in
chlorine. Write the equation of the reaction.
c) Take some antimony powder on a sheet of paper and pour it little by little into a container (jar)
filled with chlorine. Note the combustion of antimony in chlorine, obtaining a white smoke
(mixture of SbCl3 and SbCls). Write the reaction equation.
d) Cut a piece of sodium metal (the size of a pea); dry it with filter paper, put it on an iron spoon,
cover it with asbestos, heat the spoon until the sodium melts and then put it in a container filled
with chlorine. Observe the combustion of sodium in chlorine. Write the reaction equation.
3. Reciprocal action of chlorine with hydrogen.
a) Fill a dry test tube with chlorine. Fill another test tube with hydrogen from Kip's apparatus.
Holding the second test tube with the mouth down, place it over the mouth of the first test tube
containing the chlorine. Mix the gases in them by inverting the test tubes several times. After
stopping the test tubes bring their mouths close to the flame of the lamp. The crack will happen.
Immediately after the reaction, pour a little water into one of the test tubes: shake it and test the
reaction of the solution formed with litmus paper.
b) At the bottom of a dry, preheated test tube, place a piece of filter paper moistened with
turpentine. Send a stream of chlorine into the test tube, inserting (immersing) the gas pipe to the
bottom of the test tube. Note the carbonization of the turpentine and the formation of a white smoke
(often accompanied by a flame). Explain the reaction of chlorine with turpentine, bearing in mind
that turpentine consists mainly of a substance with the composition C10H16. Write the reaction
equation.
4. Chlorine water and its properties
a) Half fill a test tube with water and saturate it with chlorine. Test this chlorine water by mouth
and nose. (carefully.)
52
b) Pour small amounts into three test tubes, in the first indigo solution, - in the second fuchsia
solution, and in the third water, stained with writing ink (purple). Pour a few drops of chlorine
water into the three test tubes and shake them. Note the disappearance of the colors of the solutions.
c) Add a few drops of sodium hydroxide to a test tube containing chlorine water, shake and
smell. Explain the disappearance of chlorine smell. Write the reaction equation.
d) Pour some water into a test tube, and after inserting it (immerse it in snow or ice with table salt,
saturate it with chlorine. Observe the formation of yellow crystals with the composition Cl2.
8H2O. Remove the test tube with the crystals from the cooling mixture and heat by hand. Note the
melting of the crystals.
5. Preparation and properties of hydrochloric gas
Pour 2-3 g of table salt into a test tube and add up to 1/4 of its volume of concentrated sulfuric acid
(carefully). In the mouth of the test tube, put the stopper with the tube for removing the gas, then
fix it (the test tube) obliquely on the tripod.
Insert the degassing tube into a dry test tube almost all the way to the end. Close the mouth of the
dry test tube with a piece of loose cotton. Place a glass of water nearby.
Gently heat the test tube containing the salt with sulfuric acid. When abundant white smoke
appears above the mouth of the cotton-capped test tube, stop heating. Remove the cotton and
immediately close the mouth of the test tube with your finger.
Turn the test tube upside down and dip the mouth of the test tube into the glass of water you have
nearby. After removing the finger, notice the rise of the water level in the test tube. Explain the
reason.
Close the test tube under water with your finger and remove it from the water. Test the digestion
with a blue litmus paper. Write the equation for the reaction of NaCl with H2SO4.
To a portion of the above solution add a few drops of silver nitrate solution. Note the formation of
a white silver chloride precipitate. Write the reaction equation.
b) Take some solution of any soluble chloride (of any metal) in a test tube and add a few drops of
silver nitrate. Note the formation of silver chloride precipitate. Write the reaction equation.
Lab 10-BORON, ALUMINUM, CARBON AND SILICON.
Carbon belongs to group IV A of the periodic system. In addition to carbon, this group includes
silicon, germanium, lead and tin. The atoms of all these elements in the outer shell have 4 electrons
each. These are able to give up these electrons or gain four more.
Carbon is a typical metalloid. In its compounds, it has negative valence (-4) and positive valence
(2 and 4).
53
With hydrogen, carbon forms a large number of compounds called hydrocarbons. The simplest of
these compounds is methane CH4, which is a colorless, odorless, slightly soluble gas in water
(about 4 volumes of CH4 dissolve in 100 volumes of water under normal conditions). Under
normal conditions, methane is a chemically inert substance. If ignited, it burns with a pale light
blue flame forming CO2 and H2O. Methane forms explosive mixtures with air.
In the laboratory, methane is usually prepared by heating anhydrous sodium acetate and soda lime
(mixing NaOH with Ca(OH)2).
CH3 COONa+NaOH=Na2CO3+CH4
Another representative of hydrocarbons is acetylene C2H2. This is a colorless gas, with a weak
characteristic smell, it dissolves quite well in water (in 1 volume of water under normal conditions,
one volume of acetylene dissolves). In air, acetylene burns with a sooty flame that emits a strong
light. Its mixture with oxygen or air is highly explosive. Acetylene is produced by the interaction
of calcium carbide (carbide) with water.
With oxygen, carbon forms oxides: carbon dioxide (carbon dioxide) CO2 and carbon
monoxide CO.
Carbon dioxide is a colorless gas with a weak sour taste, it is 1.5 times heavier than air. It dissolves
quite well in water. In a volume of water under normal conditions, 1 volume of carbon dioxide is
dissolved. Carbon dioxide does not burn and does not help burn ordinary fuels. Alkaline metals,
magnesium and glowing phosphorus continue to burn even in carbon dioxide.
In the laboratory, carbon dioxide is prepared by the action of acids on the marble (CaCO3).
When dissolved in water, CO2 partially acts on it to form carbonic acid, which is known only in
digestion; during the heating of the latter, H2CO3 decomposes into water and carbon dioxide.
Carbonic acid is a very weak acid and dissociates to a small degree into the H+ ion and HCO3
which are formed in very small amounts. So in the aqueous solution of CO2 there are the following
balances:
Carbonic acid, as a dibasic acid, forms two types of salts: normal salts (carbonates) and acid salts
(hydrocarbonates).
Sodium, potassium and ammonium carbonate as well as almost all hydrogen carbonates are soluble
in water (carbonates of other metals are insoluble).
Alkaline metal carbonates in aqueous solutions are hydrolyzed and give an alkaline reaction:
All carbonic acid salts are decomposed by strong acids releasing carbon dioxide, while during
heating almost all these salts decompose into metal oxide and carbon dioxide. (Only Na2CO3 and
K2CO3 can melt without decomposing). Carbon monoxide is a colorless, odorless, extremely
poisonous gas that is slightly lighter than air. Carbon monoxide is slightly soluble in water (about
2.5 volumes in 100 volumes of water under normal conditions). In air, CO burns with a blue flame.
At high temperatures this is a good reducer.
54
In the laboratory carbon monoxide is prepared by removing water from oxalic acid H2C2O4 or
from formic acid HCO2H by means of concentrated sulfuric acid:
Apparatus and containers: 1) technical-chemical scale with weight box; 2) apparatus according
to figure 75; 3) apparatus according to fig. 76; 4) apparatus according to picture 77; 5) apparatus
according to fig. 62; Kip's camera; 7) measuring cylinder with 100 ml pupil; 8) lamp; 9) porcelain
mortar and pestle; 10) glasses (or containers) with heat 250 ml 2 pieces; 11) test tube holder; 12)
pliers; 13) iron spoon; 14) funnel bent with a right angle; 15) glass birch; 16) pot 0.5-1; 17) burette;
18) rubber stopper; 19) rubber hoses; 20) test tubes.
1) magnesium (bar); 2) red phosphorus; 3) barium carbonate BaCO3; 4) calcium carbide CaC2; 5)
calcium carbonate CaCO3; 6) marble CaCO3; 7) magnesium carbonate MgCO3; 8) basic copper
carbonate Cu2(OH)2CO3; 9) sodium bicarbonate NaHCO3; 10) anhydrous sodium carbonate
Na2CO3.11) Sodium acetate CH3COONa (melted); 12) lime with sodium soda; 13) ethyl alcohol
C2HsOH; 14) oxalic acid H2C2O4; 15) litmus paper; 16) cotton; 17) birch wood (pine); 18
manganese dioxide MnO2; 19) acetone CH3COCH3; 20) sugar. digestion; 1) sulfuric acid H2SO4
(concentrated) 2) hydrochloric acid HCl (with concentrations 1:4 and 2 normal) 3) acetic acid
CH3COOH (2 normal); 4) ammonium hydroxide NH4OH (2 normal); 5) calcium hydroxide
Ca(OH)2 (saturated); 6) aluminum sulfate, Al2(SO4)3 (0.5 normal); 7) potassium carbonate
K2CO3 (2 normal); 8) copper sulfate CuSO4 (0.5 normal); 9) sodium hydrogen carbonate; 10)
silver nitrate AgNO3(1 normal); 12) litmus.
1. Combustion of methane in air and chlorine
a) After opening the cylinder containing the methane obtained in the previous experiment, ignite
the gas with the flame of a lighted wooden birch. Methane burns with a dull flame without soot.
To keep burning continuously, expel the gas by pouring water into the cylinder. Write the reaction
equation.
b) Fill a test tube with methane up to 1/3 of its volume, while the remaining volume is filled with
chlorine. Close the test tube with your finger and shake it several times to mix the two gases as
well as possible. Open the mouth of the test tube and insert a lighted but non-flaming wooden birch
into it. Note the vigorous combustion and soot separation. Write the reaction equation.
2. Preparation and burning acetylene
Put 1-2 pieces of calcium carbide in a test tube and pour 1-2 ml of water. Immediately, the rapid
formation of gas begins. Since calcium carbide is technical, the acetylene obtained appears mixed
with various impurities, which give it a bad smell. Write the reaction equation.
When you have expelled the air from the test tube (approximately 1 minute after the reaction has
started), ignite the gas that is released near the mouth of the test tube. Acetylene burns with a
bright, sooty flame. Blow toward the acetylene flame. Soot disappears (Why?). Write the equations
for the reactions of complete combustion and incomplete combustion of acetylene.
55
3.Preparation carbon dioxide
The tip of the funnel must reach the bottom of the pot. In the latter place pieces of marble or
limestone and dilute hydrochloric acid (1:4) through the funnel. Fill three containers (or glasses)
with the carbon dioxide that is released and cover them with cardboard or a sheet of paper.
The filling of the container with carbon dioxide can be understood by the extinguishing of the
burning birch as it approaches the mouth. Write the reaction equation. Save the containers
containing the carbon dioxide for future experiments.
4. Pouring carbon dioxide from one container to another
Place a small piece of cotton soaked in alcohol in a glass and light it with the side of a burning
birch. Then carefully pour into it (as water) the carbon dioxide from one of the glasses filled in the
previous experiment. The burning of alcohol is stopped.
The lit birch, inserted into the glass from which the carbon dioxide has been poured, continues to
burn.
5. Combustion in carbon dioxide
a) In a beaker filled with carbon dioxide, insert a magnesium strip heated in air, holding it with
forceps. Magnesium continues to burn in the carbon dioxide forming white magnesium oxide and
black soot grains. Add a little diluted hydrochloric acid to the formed products and shake them.
Will both products dissolve? Write the equations of the reactions.
b) Light some red phosphorus in a small iron spoon and put it in a beaker of carbon dioxide.
Phosphorus continues to burn. Write the reaction equation.
6. Solubility of carbon dioxide in water
Fill the test tube 1/4 full with water, add a little blue litmus solution, and bubble through it a
stream of carbon dioxide. Note the color change of the litmus. Write the reaction equation. Boil
the digestate. Explain the change that occurs in its color.
7. Formation of carbonic acid salts
a) Bubble a stream of carbon dioxide into a test tube with lime water (with Ca(OH)2 solution).
Note the formation of a white precipitate. This reaction is usually used to dictate carbon dioxide.
Continue delivering CO2 until the precipitate dissolves. Write the equations of the reactions.
Divide the obtained solution into two test tubes. Heat one test tube, while adding lime water to the
other. In both cases, a white precipitate is separated. Write the equations of the reactions.
8. Hydrolysis of carbonic acid salts
a) test the dissolution of NaHCO3, Na2CO3 and K2CO3 with an almost neutral alkane, in the
second and third it shows a strong alkaline reaction. Explain these phenomena. Write the equations
of the hydrolysis reactions.
56
b) Pour some CuSO4 solution into a test tube, while adding Na2CO3 solution to the Al2(SO4)3
solution and then to both test tubes. Blue-colored Cu2(OH)2CO3 and white-colored Al(OH)3
precipitates are formed, respectively. In both cases, carbon dioxide is released. Write the equations
of the reactions.
9. Action of acids on carbonates
In one test tube pour some MgCO3, while in another test tube take BaCO3. Then add dilute
hydrochloric acid to both test tubes. Note the dissolution of the salts and the release of a gas. prove
that this is carbon dioxide. Write the equations of the reactions.
b) Test the solubility of the same salts in dilute CH3COOH. Write the equations of the reactions.
Explain why carbonates that are insoluble in water also dissolve in acetic acid, a weak acid.
10. Decomposition of carbonate salts during heating
Set up an apparatus according to figure 78. Pour basic copper carbonate Cu2(OH)2CO3 into the
test tube. The funnel through which the delgas is inserted into a test tube containing lime water.
Heat the test tube containing the salt. Note the discoloration of the basic copper carbonyl and the
turbidity of the lime water. After the reaction, black copper oxide remains in the test tube. Write
the equations of the reactions. Do similar experiments taking NaHCO3, Na2CO3 and CaCO3.
Infer which of these studied salts is the most stable to heat.
Silicon
Silicon is an element of group IV A of the periodic system. In the outer layer of its atom, as well
as in that of carbon, there are 4 electrons. The radius of the silicon atom is greater than that of the
carbon atom, so it accepts electrons more weakly.
In its compounds, silicon almost always has a valence of 4 (positive or negative).
Silicon belongs to the metalloids, but its metalloid properties are weaker than those of its analogue,
carbon.
Amorphous silicon, with a brown color, and crystalline silicon with a gray color are known.
In its free state, silicon is a chemically less active element and reacts with other elements (with the
exception of fluorine) only when heated. With some metals (Mg, Ca, Fe, etc.) it forms chemical
compounds called silicides.
Acids do not act on it. Alkalis, even very diluted ones, dissolve silicon forming salts of silicic acid
and extracting hydrogen according to this equation:
Si+2NaOH+H2O=Na2SiO3+2H2H2 O=Na2SiO3+2
Salts of silicic acid with weak bases, eg (NH4)2SiO3, are completely hydrolyzed.
57
Silicates are almost all colorless, melt with great difficulty and do not dissolve in water. Soluble
sodium and potassium silicates are called "soluble glass" and their aqueous solutions are called
"liquid glass".
During the interaction with halogens, silicon forms SiF4, SiCl4, SiBr4. Silicon fluoride is also
produced, by the action of Hf on SiO2. Under ordinary conditions, this represents a colorless gas
with a strong odor, fuming in the air, because with water vapor it undergoes hydrolysis to form
SiO2 (exactly SiO2H2O) and Hf.
Apparatus: 1) technical-chemical balance and weight box; 2) Kip's apparatus, filled with marble
and hydrochloric acid (1:1); 3) tripod with clips; 4) lamp; 5) porcelain mortar and pestle; 6)
student's glass 250 ml-2 pieces; 7) funnel; 8) test tube holders; 9) copper birch.
Reagents and materials: 1) magnesium (powder); 2) quartz (dust) or sea sand; 3) sodium
hydroxide NaOH, calcium fluoride CaF2, 5) filter paper; 6) litmus paper; 7) glass pipes; 8) sulfates
of Cu, Mn, Ni, Cr, Co; 9) Al and Fe shapes, 10) silica gel with a diameter of 0.25-0.5 mm.
Solutions: 1) concentrated sulfuric acid H2SO4; 2) concentrated hydrochloric acid HCI and 1:1;
3) sodium hydroxide NaOH (40%) 4) ammonium chloride NH4C1 (saturated); 5) sodium silicate
Na2SiO3 (concentrated); 6) phenolphthalein; 7) ammonium hydroxide (concentrated).
1. Preparation of amorphous silicon
Pour into a test tube a little mixture of magnesium powder and finely ground quartz (7:10 weight
ratio). In the absence of quartz, you can use clean sand. Fix the sample on the stand vertically. First
heat the mixture quickly and then heat the end of the test tube until the mixture melts. After that,
remove the lamp, because the reaction takes place with the release of a large amount of heat.
Sometimes you need to continue the heating for 2-3 minutes and only after that, turn it on. Observe
the phenomena that take place and write the reaction equations, bearing in mind that in addition to
magnesium oxide and silica, a small amount of magnesium silicate Mg2Si is also obtained.
After cooling, break the test tube in a mortar and pour the obtained mass into small pieces in a
glass containing diluted hydrochloric acid (1:1). In this case MgO dissolves. Mg2Si reacts with
HCl, forming compounds of silicon with hydrogen, silanes, while silicon in the form of a brown
powder remains at the bottom of the glass. The silanes formed burn near the surface of the liquid
with a characteristic crackle, forming a white SiO2 fume. Write the equations of the reactions.
After the completion of the reaction pour off the liquid, rinse, filter, dry the bottom and check the
amorphous silicon obtained. Based on the experiment, draw a conclusion about how silicon
behaves with dilute acids.
2. Interaction of silicon with alkalis
Without the amorphous silic, obtained in the previous experiment, pour it into a test tube where
you add 2-3 ml of concentrated alkaline solution and heat it. Note the dissolution of the silica and
the release of a gas. Prove that the gas released is hydrogen. Write the reaction equation.
3. Preparation of silicic acid hydrogel
58
To 5 ml of the concentrated solution of sodium silicate add 2-2.5 ml of diluted hydrochloric acid
(1:1) and mix the solution well with a glass rod. Due to the formation of silicic acid, the entire
content of the test tube turns into a gelatinous mass. Write the reaction equation.
4. Preparation of silicic acid hydrosol
Add a little concentrated hydrochloric acid to 3-5 ml of sodium silicate solution. As a result, a
colloidal solution of silicic acid is obtained. Bring the solution to a boil. Note the formation of
silicic acid gel.
5. Extraction of silicic acid from its soluble salts
Collect a stream of carbon dioxide from Kip's apparatus in dissolving the sodium silicate. Note the
formation of silicic acid. Write the reaction equation.
Which of the acids: H2SiO3 or H2CO3 is the stronger electrolyte?
6. Absorbent properties of silica gel
Take 15-20 drops of copper sulfate solution in a large test tube and drop into it aqueous ammonia
solution until no more complex salt (cupratetetramine sulfate) is formed, i.e. until the dark blue
color of the solution no longer forms. Pour about 2 g of silica gel powder with a diameter of 0.25-
0.5 mm into the obtained solution and mix for a long time. The colorless silica gel powder will
absorb the complex and turn dark blue, while the color of the solution will fade. Pour the solution,
while rinsing the colored silica gel 3-4 times with 2 ml of hydrochloric acid, mixing and decanting.
The silica gel will lose its blue color because the acid dissolves (destroys) the complex.
Boron and aluminium
Boron and aluminum are typical elements of group III A of the periodic table. Their atoms have 3
electrons in their outer shell. Both of these elements show the same positive valence 3, but they
have many differences from each other.
Boron is a metalloid, although its metalloid properties are rather weakly demonstrated. In terms of
properties, boron is more similar to silicon.
Free boron is produced by reducing boric anhydride B2O3 with metallic magnesium. In this case,
boron is separated in the form of an amorphous powder with a purple color.
The most important compounds of boron from a practical point of view are boric acid and borax.
Boric acid (more precisely orthoboric acid) H3BO: is formed by the union of boric anhydride with
water. It is a white crystalline substance that dissolves with difficulty in cold water, but dissolves
very well in hot water. During heating, H3BO3 releases water and transforms first (at 100C) into
metaboric acid HBO2 and then (at 140℃) into tetraboric acid H2B4O7 and finally into boric
anhydride. When dissolved in water, all these substances attract water and turn into boric acid
H3BO3. Boric acid is one of the weakest acids. Its salts are called borates.
59
Borax Na2B4O7. 10H2O is white crystalline substance. Boric acid can be extracted from borax
by acting with any strong acid:
Borax is characterized by the ability to form colored pearls when heated with the salts of some
metals. During heating, borax loses its water of crystallization and melts forming a transparent
mass like glass. By fusing with metal oxides, anhydrous borax forms double salts, colored with a
characteristic color, for example:
Because of its ability to form colored pearls, borax is used in analytical chemistry to detect certain
metals (chromium, cobalt, etc.).
Fluorine compounds (volatile) of boron color the lamp flame green.
Aluminum in the free state is a silver-white metal. It does not oxidize at ordinary temperature, in
the air, because it is quickly covered with a thin and strong oxide layer, which protects it from
further oxidation. This layer is removed by amalgamation (amalgams are liquid or solid alloys of
metals with mercury). Thanks to the presence of the protective layer of aluminum oxide, it does
not interact with water, so it does not release hydrogen from water. But if aluminum that does not
have a protective layer is thrown into water, then it will release hydrogen from the water and turn
into Al(OH)3. Aluminum in dilute hydrochloric and sulfuric acid dissolves easily, especially when
heated. It also dissolves easily in alkali solutions, forming aluminates, for example:
2Al+2NaOH+2H2O=2 NaA102+3H2
This reaction takes place in two stages:
1) 2Al+6H2O=2Al(OH)3+3H2;
2) 2Al(OH)3+2NaOH=2NaA102+4H2O
Cold nitric acid does not dissolve aluminum, but makes it "passive" against hydrochloric and
sulfuric acid.
At high temperatures, aluminum energetically frees metals from their oxides for example:
2Al+Fe2O3=Al2O3+2Fe.
Aluminum forms only one oxide Al2O3 which is called aluminum oxide. Aluminum oxide Al2O3
and its hydroxide Al(OH)3 have amphoteric properties. Al(OH)3 dissolves in both acids and
alkalis, forming salts called aluminates in the latter case. We distinguish two forms of aluminates:
metaaluminates NaAlO2 and sodium orthoaluminates Na3AlO3.
Aluminum salts, formed by strong acids due to hydrolysis, give an acid reaction in aqueous
solutions. Some aluminum salts, for example Al2S3 or Al2(CO3)3 in aqueous solutions are
completely hydrolyzed. Aluminates are also hydrolyzed. The least stable aluminate is sodium
aluminate whose solution when heated completely dissociates to form aluminum hydroxide.
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Of the aluminum salts, the most important from the technical point of view is the double sulfate
of aluminum and potassium KAI(SO4)2 12H2O, (alum of aluminum and potassium). This salt is
used as a dyeing agent for cotton fabrics.
Apparatus and containers: 1) technical-chemical scale with weight box; 2) tripod with ring; 3)
bulb; l 4) lamp; 5) iron fence; porcelain triangles; 6) porcelain mortar; 7) funnel; 8) glass rod with
platinum or nickel-chrome wire; 9) glass with heat 100 ml; 10 metal pliers; 11) test tube holder;
12) asbestos fibers; 13) firing funnel (refractory); 14) bottle with two mouths; 15) distillation pot;
16) separating funnel; 17) rubber stoppers, 18) desiccant bottles.
1) magnesium (powder); 2) aluminum (plates, sawdust and powder) 3) sodium tetraborate

Na2B4O7. 10H2O (borax); 4) boric acid H3BO3; 5) litmus paper; 6) filter paper; 7) cover letter;
8) cotton, 9) writing ink in different colors; 10) potassium permanganate KMnO4.
Solutions: 1) nitric acid HNO3 (concentrated and 2 normal); 2) sulfuric acid H2SO4 (concentrated
and 2 normal); 3) hydrochloric acid HCI (concentrated and 2 normal); 4) sodium hydroxide NaOH
(30% and 2 normal); 5) sodium tetraborate Na2B4O7 (saturated); 6) cobalt chloride COCl2
(concentrated); 7) mercury chloride HgCl2 (0.5%); 8) mercury nitrate Hg2(NO3)2(0.2 normal); 9)
aluminum sulfate Al2(SO4)3 (0.5 normal); 10) sodium acetate CH3COONa (0.5 normal); 11)
ammonium chloride NH4Cl(2 normal); 12) ammonium sulfide (NH4)2S.
Practical work
1. Preparation of amor horn
(Do this work in the gas closet)
a) Put some boric acid in an iron pot, heat it, over the lamp and first carefully scrape it, then harden
it.
Note the formation of boric anhydride. Write the reaction equation. After cooling, take the obtained
mass of boric anhydride out of the pot, press it carefully in a mortar, weigh it and mix it with a
double amount of magnesium powder.
Pour this mixture into the pot, place it in the gas cupboard and heat it over the lamp. Watch the
development of the reaction through the glass lowered below the gas cabinet. After cooling, pour
the obtained mass in a beaker and work with warm hydrochloric acid to dissolve the MgO.
Amorphous boron remains in the turbidity, a dark brown powder. Filter the boron powder. Write
the reaction equations.
b) Act on a small amount of boron powder by dissolving some alkali. Compare the behavior of
boron and silica towards alkali dissolution.
2. Preparation and properties of boric acid
61
a) Carefully pour into a test tube, containing the saturated solution of borax, concentrated sulfuric
acid. Cool the test tube containing the mixture in a stream of cold water to reduce the solubility of
the H3BO3 obtained. Note the separation of white crystals of H2BO3. Write the reaction equation.
b) Test the degree of dissolution of H3BO3 crystals in cold and warm water.
c) Dissolve a small amount of boric acid in water and test the dissolution with a blue litmus paper.
Is boric acid a strong or weak acid?
d) Heat the platinum wire in the flame of the lamp and touch the powdered H3BO3 with it. Heat
the wire with the dust attached to it again near the edge of the outer cone of the lamp flame. Note
the characteristic green coloration of the flame.
3. Properties of borax
a) Test the dissolution of borax with blue and red litmus paper. Write the equation for the
hydrolysis reaction.
b) Pick up some borax crystals with the tip of the platinum or nichrome wire and insert them into
the flame of the lamp. Note the formation of the translucent, vitreous-looking borax pearl.
c) Immerse the obtained borax pearl in the concentrated cobalt salt solution and heat again. Note
the blue coloration of the pearl. Write the reaction equation.
Instead of cobalt salt, you can get trivalent chromium chloride. In this case the pearl will turn
green.
4. The connection of aluminum with oxygen
Clean an aluminum plate with sandpaper. Mb: put a drop of Hg2 (NO3)2 or HgCl2 on the cleaned
metal surface (these solutions are poisonous). When the surface of the metal under the mercury
salt solution has turned ash-colored, due to the formation of amalgam, shake the solution point and
wipe the wet area lightly with cotton or filter paper. Let the metal stand in the air. Note the
formation of the fluffy white hair of Al(OH)3 and the heating of the plate. Write the equations of
the reactions.
5. The interaction of aluminum with water
put some powder or aluminum shavings in a test tube and add 2-5 ml of water. You will see that
no reaction will take place. Add 2-3 ml of dilute NaOH solution to the test tube and boil the sawdust
together with the alkali to remove the protective layer. After that pour the liquid, rinse the flour
several times with water to remove the alkali and let it stand in the water. Note the gas (hydrogen)
bubbles coming out. Write the reaction equation.
6. Interaction of aluminum with acids
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a) Put 2 normal solutions of acids into three test tubes; in the first solution of hydrochloric acid, in
the second of sulfuric acid and in the third of nitric acid. Pour some aluminum powder (or
aluminum shavings) into each test tube.
The reaction will proceed more energetically with hydrochloric acid and much more slowly with
sulfuric acid. Whereas with dilute nitric acid, aluminum will not react.
b) (Do this experiment in the gas cabinet). Pour aluminum filings into a test tube containing a small
amount of concentrated HNO3 (specific gravity 1.4). In the cold, aluminum does not dissolve,
because its surface is covered with a protective membrane. Heat the solution and notice at first the
slow development and then the rapid development of the reaction. Write the reaction equation.
7. Interaction of aluminum with iodine
Mix 0.1 g of aluminum powder with 1-2 g of crushed dry iodine on an asbestos grid. Shape the
mixture into a cone with a dimple at the top. Using a dropper, pour 2-3 drops of water into the
hole. After a few seconds, notice the rapid reaction accompanied by the release of violet vapors of
iodine.
Write the equations of all reactions.
8. The interaction of aluminum with alkali
Pour 3-5 ml of 30% sodium hydroxide solution into a test tube, then add some aluminum shavings.
Note the formation of hydrogen. Write the reaction equation.
9. The amphoteric character of aluminum hydroxide
Add the sodium hydroxide solution dropwise to the aluminum salt solution in a test tube until a
white gelatinous precipitate of Al(OH)3 forms. Write the reaction equation in molecular form and
in ionic form. Shake the produced precipitate and divide the liquid together with the precipitate in
half into two test tubes. Add dilute hydrochloric acid to one and sodium hydroxide solution to the
other until the precipitate dissolves. Write the equations of the reactions in molecular form and in
ionic form.
10. Hydrolysis of aluminum salts
a) Test the dissolution of aluminum sulphate with red and blue litmus paper and conclude on the
hardness of aluminum hydroxide as a base. Write the equation for the hydrolysis reaction.
b) To the solution of aluminum sulfate, add the solution of ammonium sulfide. Filter the obtained
precipitate and rinse it with water on the filter. By adding diluted hydrochloric acid to the
precipitate, prove that the precipitate is not aluminum sulfide.
The precipitate is aluminum hydroxide. You can be convinced of this by treating one part of the
precipitate with hydrochloric acid and the other part with sodium hydroxide solution. In both cases,
dissolution of the precipitate will occur. Write the equations of the reactions.
63
c) Add the sodium acetate solution to the aluminum sulfate solution. No precipitate is formed in
the cold. Boil the solution and note the deposition of basic aluminum acetate precipitate Al(OH)2
(CH3COO). Write the reaction equations.
d) Add little by little NaOH to the solution of aluminum sulfate until the precipitate formed at the
beginning is dissolved. To the obtained solution of sodium aluminate, add the solution of NH4Cl
and heat. Note the deposition of Al(OH)3 precipitate and the formation of gas (determine the odor).
Write the equations of the reactions.
Lab 11-ALCALINE METALS. MAGNESIUM AND ALKALINE EARTH METALS
Alcaline Metals
Alkaline metals are the elements of group I A of the periodic system; lithium, sodium, rubidium
and cesium. Atoms of these elements in the layer. the outer ones have one electron each. During
chemical reactions, they easily release this electron and appear as energetic reducers. Their activity
increases with increasing atomic radii, that is, from lithium to cesium.
Alkali metals are easily oxidized in air, so they are stored in kerosene containers. If heated in air,
they catch fire and burn forming peroxides with the exception of lithium which forms the oxide
Li2O. Alkaline metal peroxides have this composition: Na2O2, K2O4, Rb2O4, Cs2O4.
Peroxides when interacting with water form metal hydroxides and release free oxygen, for
example:
Alkali metal oxides (with the exception of Li2O) can only be produced indirectly (for example by
heating peroxides with the corresponding metals).
All alkali metals react with water at room temperature. The reactions proceed by forming the
corresponding hydroxides and releasing hydrogen. Alkaline metal salts, with few exceptions,
dissolve well in water.
Of greater practical importance are sodium and potassium compounds: Among the most important
compounds of sodium are included: Na2CO3, NaCl NaOH and NaNO3.
Soda is one of the most important products of the heavy chemical industry. It is mainly produced,
based on the ammonia method, the basis of which are the following reactions:
Of the potassium compounds, the most important are KNO3, K2CO3, KOH and KCl.
The caustic alkalis NaOH and KOH in industry are produced by electrolysis of chloride solutions
or by another older method, boiling the solution of carbonates with lime sorbet.
Apparatus and containers: 1) technical-chemical scale with weight box; 2) Kipp's apparatus,
charged to obtain CO2; 3) tripod with rings; 4) lamp; 5) measuring cylinder with 100 ml pupil; 6)
glass cylinder with pupil 200 ml; 7) porcelain bowl; 2 pieces; 8) porcelain bowl; 9) porcelain
triangle; 10) knife; 11) tweezers; 12) chemical glasses with pupils 150-200 ml 2 pieces; 13) funnel;
64
14) glass birch with platini or nichrome wire; 15) glass birch; 16) asbestos mesh; 17) test tube
holder; 18) test tubes.
1. sodium; 2) potassium; 3) sodium peroxide Na2O2 (powder); 4) Sodium chloride NaCl; 5)

potassium carbonate K2CO3; 6) ammonium carbonate (NH4)2 CO3; 7) slaked lime Ca(OH)2; 8)
litmus paper; 9) filter paper; 10) wooden sticks.
Solutions: 1) hydrochloric acid HCl (2 normal); 2) sodium chloride NaCl (2 normal); 3) potassium
chloride KCl (2 normal); 4) lithium chloride LiCl (2 normal); 5) litmus; 6) phenolphthalein
(alcoholic) 7) potassium dihydrogenantimonate KH2SbO4(2 normal); 8) sodium acid tartrate
NaHC4H4O6(2 normal);9) sodium hexatrocobaltate (III) Na3[Co(NO2)6](2 N);10 sodium
carbonate Na2CO3(2 N); potassium phosphate K3PO4(2 N)
Practical work
1. Sodium burning
(Do this work behind the glass of the gas cabinet) From a container containing sodium and
kerosene, remove with tweezers a piece of metallic sodium; place on a filter paper and cut off with
a knife a piece about the size of a pea. Dry the metal well on the surface by means of filter paper,
place it in a porcelain cup and heat it carefully on the triangle behind the glass of the gas cupboard,
in the small flame of the lamp. As soon as the sodium has caught fire, remove the lamp. Observe
the burning of the sodium in the cup and the sodium peroxide. Na2O2 formed. Write the reaction
equation.
2. Action of alkaline metals with water
(Do this work behind the glass of the gas cabinet).
a) Take a porcelain bowl half filled with water, cut a small piece of sodium with a knife (the size
of half a pea), dry it with filter paper and drop it into the bowl of water. Observe the progress of
the reaction through the glass of the fume hood. Glass protection is necessary because sodium
sometimes interacts with fractured water. When the reaction is complete, test the solution obtained
by means of a colander or by means of phenolphthalein. Write the reaction equation.
b) Repeat the previous experiment using potassium. Take a very small piece of metal for the
experiment because potassium reacts with water much more energetically than sodium. Note the
interaction of potassium with water. Write the reaction equation.
3. Interaction of sodium peroxide with water
In a test tube containing a small amount of water add some Na2O2 powder. By inserting a burning
wooden stick into the test tube, prove that oxygen is released during the reaction. After the
experiment is over, test the dissolution with litmus paper. Write the reaction equation.
4. Cooking soda using the ammonia method
65
Dissolve 30 grams of NaCl in 100 ml of water and add 25 grams of (NH4)2CO3 dissolved in as
little water as possible to the obtained solution. Pour this mixture into a tall glass cylinder and
collect a strong stream of CO2 through it.
After some time (15 minutes) the liquid becomes cloudy and a fine precipitate of NaHCO3 begins
to separate from it.
Filter off the precipitate and rinse the filter with a small quantity of cold water. Pour the precipitate
into a previously weighed porcelain pot, and after it has first been dried by carefully heating it,
twirl it over the gas lamp until the weight remains unchangeable. By determining the weight of the
obtained soda, calculate the percentage of its benefit. Compare this with the theoretical percentage.
5. Preparation of potassium hydroxide from its carbonate.
Pour 10 ml of water into a glass and dissolve 10 grams of potassium carbonate in it. Heat the
solution until it boils and add little by little mixing 8-10 g of slaked lime. Boil this solution by
constantly adding water so that the volume of the liquid remains approximately the same until the
end of the reaction. Test if the reaction has developed to the end. For this purpose, you should take
a part of the liquid in a test tube and act on it with hydrochloric acid. After the reaction is over, let
the solution cool and separate the clear liquid from the precipitate by decantation.
Write the equation for the interaction of potassium carbonate with slaked lime.
Explain the development of the reaction from which potassium hydroxide is formed, taking into
account the solubility of CaCO3 and Ca(OH)2.
6. Reactions for the detection of sodium, potassium and lithium ions
a) Pour into a test tube containing 2-3 ml solution of any sodium salt, the concentrated solution of
potassium dihydrogenantimonate (KH2SbO4). To hasten the precipitation of sodium antimonate,
rub the inside of the test tube with a glass rod.
b) Pour into a test tube containing a solution of a potassium salt, a solution of acid sodium tartrate
(NaHC4H4O6). Rub the inside of the test tube with a glass rod for rapid precipitation of the
potassium tartrate.
Note the precipitates and write the reaction equations.
c) In a test tube containing the neutral or acidified solution with acetic acid of a potassium salt
pour the solution of sodium hexanitrocobaltate (III) Na3[(Co(NO2)6). Note the precipitation of
potassium hexanitrocobaltate (III) and sodium K2Na [CO(NO2)6], in the form of yellow crystals.
d) Pour the solution of sodium carbonate, sodium phosphate and fluoride in three test tubes each
containing 2 ml of lithium chloride solution of potassium. Heat the samples with solution, observe
the white precipitates of Li2CO3, Li3PO4 and LiF. Write the reaction equation.
7. Flame staining by sodium and potassium lithium salts
66
Clean the platinum or nichrome wire first by dipping it in concentrated hydrochloric acid and
foaming it several times. Meanwhile, insert the cleaned wire into the solution of one of the lithium
salts and then into the bright flame of the lamp. Note the intense red color of the flake.
Do this experiment with potassium and sodium salts as well. Note the violet color of the flame
from the potassium salts and the yellow color from the sodium salts.
Magnesium and the alkaline metals
Magnesium and the alkaline earth metals calcium, strontium and barium belong to group II A of
the periodic system. In the outer layer of the atoms of these elements, there are two electrons,
which are separated during chemical reactions easily. Therefore, in their compositions, Mg, Ca, Sr
and Ba have a positive valence of two. These are strong reducers. Their reducing activity increases
with increasing atomic radii, from magnesium to barium. In the free state these are light non-
ferrous metals white as silver. Calcium, strontium and barium dissolve water at ordinary
temperature, while magnesium in the cold acts with water much more slowly, but when heated it
acts more energetically.
During the combustion of magnesium and alkaline earth metals, oxides with the composition MeO
are produced, which are directly connected to water, forming hydroxides with the composition Me
(OH)2.
Magnesium hydroxide does not dissolve well in water, but readily dissolves in ammonium salts
by reacting with and forming the weak base NH4OH e.g.
Mg(OH)2+2NH4CI=MgCl2+2NH4OH
Alkaline earth metal hydroxides dissolve in water quite well and give strong bases. The increase
in the basic character and in parallel with the increase in solubility in water, increases from calcium
hydroxide to barium hydroxide.
Many salts of magnesium and alkaline earth metals do not dissolve well in water. During the action
of soda on the dissolution of magnesium, calcium, strontium and barium salts, insoluble carbonates
are produced (magnesium forms basic carbonate, while other metals form normal carbonates).
The hydrogen carbonates of all four metals dissolve well in water. Of the sulfates, MgSO4
dissolves easily in water, CaSO4 dissolves with difficulty. SrSO4 and BaSO4 are strictly insoluble
in water and even in acids.
Water hardness depends on the amount of soluble calcium and magnesium salts in natural water.
Calcium and magnesium are found in water, mainly, in the form of soluble hydrogen carbonates,
as well as in the form of sulfates, chlorides and nitrates.
During the boiling of water, Ca (HCO3)2 and Mg(HCO3)2 are transformed into normal insoluble
salts, which precipitate and in this way, the hardness caused by these salts is removed. This water
hardness is called eliminable or temporary. Hardness which cannot be removed by boiling is called
durable. It is mostly caused by sulfates and chlorides of calcium and magnesium.
67
Hard water forms with soap insoluble salts of fatty acids. The greater the hardness of the water,
the more soap is needed to produce a stable foam. One of the methods of determining the hardness
of water is based on this.
Volatile salts of alkaline-earth metals give the lamp flame its characteristic color.
Apparatus and vessels: 1) Kipp's apparatus, charged for cooking CO2; 2) lamp; 3) measuring
cylinder with 10 ml pupil; 4) pot with flat bottom heat 500-100 ml; 5) glass rod with platinum or
nickel-chrome wire; 6) test tube holders; 7) test tubes. Reagents and materials:
1) Calcium carbonate CaCO3 (powder); 2) magnesium carbonate MgCO3 (powder); 3) litmus

paper; 4) magnesium chloride MgCl2.6H2O; 5) magnesium oxide MgO; 6) gypsum 2CaSO4.H2O.
Solutions: 1) nitric acid HNO3(2 normal); 2) sulfuric acid H2SO4 (2 normal); 3) hydrochloric
acid HCI (2 normal); 4) sodium hydroxide NaOH(2 normal), 5) ammonium hydroxide NH4OH (2
normal); 6) calcium hydroxide Ca (OH)2 (saturated); 7) magnesium sulfate MgSO4(1 normal); 8
ammonium chloride NH4C1(2 normal); 9) sodium carbonate Na2CO3 (2 normal); 10) calcium
chloride CaCl2 (1 normal); strontium chloride SrCl2 (1 normal); 12) barium chloride BaCl2 (1
normal); 13) sodium sulfate Na2SO4 (2 normal); 14) calcium sulfate CaSO4 (saturated); 15)
strontium sulfate CrSO4 (saturated); 16) soap solution (2%), 17) sodium hydrogen phosphate
Na2HPO4; 18) ammonium oxalate(NH4)2 C2O4(10%).
Practical work
1. Preparation of magnesium hydroxide
Pour into two test tubes a little solution of some magnesium salt. Then add sodium hydroxide
solution to one test tube and ammonia solution to the other. Note the color of the magnesium
hydroxide obtained. Write the equations of the reactions. Add ammonium chloride solution to the
precipitates until dissolved. Write the equation for the reaction between magnesium hydroxide and
ammonium chloride in molecular form and in ionic form. Explain the phenomenon that occurs
starting from the solubility product.
2. Hydrolysis of magnesium salts
Test the dissolution of magnesium salt with red and blue litmus paper. Write the equation of the
hydrolysis reaction. What conclusion can be drawn about magnesium hydroxide as a base?
3. Basic magnesium carbonate
Add the soda solution to the MgSO4 solution. Note the formation of a white precipitate of the
basic salt Ng2(OH)2CO3. Write the reaction equation.
Add the ammonium chloride solution to the sample. Note the solubility of the precipitate. Write
the solubility product equation of Mg2(OH)2CO3 and explain the solubility of the precipitate.
4. Formation of magnesium hydrogen carbonate
68
To a very dilute solution of any magnesium salt, add a little of the Na2CO3 solution. Note the
formation of basic magnesium carbonate.
Saturate the solution together with the precipitate with carbon dioxide coming from Kip's
apparatus. Note the slow dissolution of the precipitate due to the formation of magnesium
hydrogencarbonate, which is quite soluble in water. Write the reaction equation.
5. The reaction for the detection of the magnesium ion (Mg2+)
Pour into a test tube, containing magnesium hydroxide, ammonium chloride solution until it is
completely dissolved. Pour sodium hydrogen phosphate solution into the obtained solution.
Observe the white precipitate. Write the reaction equation.
6. Preparation of magnesium cement
Dissolve in a porcelain beaker approximately 2 g of MgCl2.6H2O in as little water as possible.

Pour into it, mixing it with glass birch crushed magnesium oxide, in such quantities that for one
part by weight of anhydrous MgCl2 correspond to two parts by weight of MgO. Put the cooked
mass (MgOHCI) in the form of a paste on a glass plate and let it solidify for you to see in the next
lesson.
7. Hydroxides of alkaline earth metals
a) To equal volumes with the same concentration of solutions of CaCl2, SrCl2 and BaCl2, taken
in separate test tubes, were added an equal amount of dilute NaOH solution. Note the amount of
precipitate formed in each test tube. Write the equations of the reactions.
b) Repeat the experiment taking instead of NaOH the aqueous solution of ammonia with the same
normality. The amount of precipitate in each test tube will be less than in the previous experiment.
Give explanations.
8. Oxalates of alkaline earth metals
To solutions of CaCl2, SrCl2, and BaCl2 in three separate test tubes, a little ammonium oxalate
solution (NH4)2C2O4 was added. Note the rate and amount of white turbidity that forms in each
test tube. Test the solubility of these oxalates in dilute acids.
Write the equations of the reactions
9. Carbonates of alkaline earth metals
In the solutions of CaCl2, SrClz and BaCl2 that are in separate test tubes, add Na2CO3 solution
little by little. Note the formation of bulky white carbonate precipitates and the change in the type
of precipitate. After heating, the carbonates fall to the bottom of the test tube in the form of small
crystals.
69
Pour diluted HCl into all the test tubes. Note the solubility of the precipitate. Write the reaction
equations.
10. Sulfates of alkaline earth metals
Produce sulfates of calcium, strontium, and barium by adding dilute H2SO4 or Na2SO2 to
solutions of the salts of these metals. Note the color of the precipitates formed. test their solubility
in hydrochloric acid and in nitric acid.
11. Comparison of the solubility of sulfates of alkaline earth metals.
a) To the solutions of CaCl2.SrCl2 and BaCl2 that are in three separate test tubes, a little of the
saturated solution of CaSO4 (gypsum water) was added. Note the formation of turbidity in the test
tubes containing BaCl2 and SrCl2. In the first test tube the turbidity appears immediately after the
addition of this solution, in the second it appears after some time. In the test tube containing CaCl2
the liquid remains transparent.
b) In this way, add the saturated solution of SrSO4 to the test tubes containing CaCl2, S-Cl2 and
BaCl2 solutions and you will see that after some time the turbidity will appear only in the test tube
containing BaCl2. Write the reaction equation.
Explain the phenomena observed in the last two experiments starting from the values of the
solubility product of CaSO4. SrSO4 and BaSO4
Lab 12-OXYGENATED COMPOUNDS OF NITROGEN. PHOSPHORUS.
Compounds of nitrogen with oxygen
The following oxides of nitrogen are known:
N2O-Nitrous oxide.NO-nitrous oxide; N2O3 nitrous anhydride.
NO2-nitrogen dioxide; N2O4 tetraoxide (tetraoxide) of nitrogen and
N2Os- nitric anhydrite. Nitric oxide and nitrogen dioxide are of the greatest practical importance
of all these oxides.
Nitrous oxide is a colorless gas that turns into a liquid with great difficulty. It is slightly soluble in
water (about 5 volumes of nitric oxide dissolve in 100 volumes of water under normal conditions).
From the point of view of chemical properties, NO is an oxide that does not form salts. It easily
combines with oxygen to form nitrogen dioxide. If liquid nitrogen dioxide is heated to +22℃, then
it will boil releasing red to brown vapors, the color of which darkens during heating.
The molecular mass of the gas is not stable, it decreases with increasing temperature. It varies
within the limits of 46 (at 150C), which corresponds to the formula NO2 to 92. which corresponds
to the formula N2O4. As the temperature decreases, NO2 (red to brown) is partially polymerized
into N2O4 (colorless) and this balance is established between these molecules:
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As the temperature decreases, the equilibrium shifts to the right. We can notice this by the change
in the color of the gas.
Nitrogen dioxide dissolves very well in water, forming two acids, nitric acid and nitrous acid:
Since nitric acid is not stable, actually the interaction of NO2 with water is based on this equation:
3NO2+H2O=2HNO2+NO
In the presence of air oxygen, the nitrogen oxide that is formed is oxidized to dioxide. Therefore
practically NO2 is completely converted to nitric acid, according to this general equation:
In the laboratory, nitric oxide is usually prepared by the action of diluting nitric acid on copper.
Nitrogen dioxide is a poisonous gas, with a red to brown color and a characteristic smell. On
cooling the color becomes pale and then condenses to a yellowish liquid, which freezes at -10C in
the form of crystals without colors.
From the dissolution of nitrogen dioxide in alkali in the presence of oxygen, salts of nitric acid
(nitrites) and nitric acid (nitrates) are formed.
Almost all nitrites (salts of nitric acid) dissolve well in water. Acids extract free nitric acid from
nitrites, which decomposes quickly:
2HNO2=NO2=NO2+NO+H2O O+H2O
Free nitric acid is unstable and only known in very dilute aqueous solutions. It has very weak
acidic properties.
Nitric acid has strong oxidizing properties, usually reducing itself to NO. On the other hand, it can
be oxidized to nitric acid under the action of stronger oxidizing substances (for example KMnO4).
Nitric acid has very pronounced oxidizing properties. It oxidizes many metalloids (S, P; etc) to the
corresponding acids. All metals, with the exception of gold, platinum and some rare metals, turn
into oxides with nitric acid. If the latter are dissolved in excess acid, then the corresponding nitrates
are formed. Fuming nitric acid (which emits fumes) practically does not act on some metals (for
example on Fe, Al), but makes them passive against acids. This is explained by the fact that a thin,
strong oxide layer is formed on the surface of the metal, insoluble in nitric acid and other acids.
The products of the reduction of nitric acid depending on the conditions (such as the concentration
of the acid, the activity of the metal, the temperature, etc.) are the various oxides of nitrogen,
nitrogen and even ammonia. Concentrated nitric acid is usually reduced to NO2; while that diluted
to NO. Highly active metals reduce dilute HNO3 to ammonia. Nitric acid belongs to strong acids.
Almost all its salts (nitrates) dissolve well in water. Nitrates are decomposed by heating, releasing
oxygen. Nitrates of the most active metals, liberating oxygen, are converted into nitrites, while
nitrates of most metals decompose to form the oxide of the metal, nitrogen dioxide and oxygen.
Under laboratory conditions, nitric acid is prepared by the action of concentrated sulfuric acid on
saltpeter.
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Apparatus and containers: 1) technical-chemical scale with weight box; 2) apparatus according
to figure 71; 3) apparatus similar to fig.72 (stand with ring and clips; lamp; lick, glass tub, asbestos
net); 4) Kip's apparatus filled with iron sulfate and hydrochloric acid; 5) tripod with rings and clips;
6) lamp, porcelain lamp; 8) funnel; 9) test tube holder; 10) test tube with stopper or glass cylinder;
11) asbestos nets; 12) pliers; 13) glass jars; 14) small pots equipped with rubber stoppers (2 pieces);
15) U-shaped glass funnel.
Reagents and materials: 1) copper (powder or sawdust); 2) tin (granulated); 3) granular zinc; 4)
aluminum (pieces); 5) sulfur (pieces); 6) potassium nitrate KNO3; 7) copper nitrate Cu(NO3)2.
3H2O; 8) sodium nitrate NaNO3; 9) pieces of wool fabric; 10) litmus; 11) filter paper; 12) birch
wood; 13) ice or snow; 14) ammonium nitrate (NH4NO3); 15) iodine (I2); 16) salt (NaCl).
Solutions: 1) nitric acid HNO3 (concentrated and diluted 1: 1); 2) sulfuric acid H2SO4
(concentrated and 2 normal); hydrochloric acid HCI (2 normal and concentrated); 4) sodium
hydroxide NaOH (2 normal); 5) barium chloride BaCl2 (1 normal); 6) potassium iodide KI (0.1
normal); 7) potassium permanganate KMnO4 (O.1 normal); 8) litmus (or fuchsia); 9) starchy
cough.
Practical work
1. Preparation of nitrous gas (gaseous gas)
a) Fill a dry test tube up to 1/3 of its volume with crystalline ammonium nitrate. Close the sample
with a stopper equipped with a funnel for the exit of gases. Heat the contents carefully at first, so
that rapid decomposition does not occur. After the air has been removed from the apparatus, collect
the released gas in two test tubes.
In the test tube filled (with gas), test whether the accumulated gas helps the burning of the lit birch.
Write the decomposition equation of NH4NO3.
b) Add nitrous oxide to the second test tube filled with nitrous gas. Note the color change in the
gaseous mixture. Write the reaction equation.
2) Preparation of nitric oxide
a) Raise the device according to figure 67 and test its kiss. Pour some copper powder or sawdust
and 5-7 ml of diluted nitric acid (1:1) into the test tube. If the reaction does not start immediately,
then heat the test tube slightly. When the air has come out of the apparatus and the gas coming out
of the tube is colored yellow-brown in the air, (Why?) start collecting it in a test tube (or in a
cylinder) above the water. After filling the test tube with nitrous oxide, close it with a stopper and
save it for the next experiment. Write the reaction equation.
b; Filter the colored solution that remains in the tube of the apparatus after removing the acetic
oxide. Collect the filtrate in a porcelain beaker and concentrate by evaporation in a water bath.
Allow the concentrated solution to cool and then observe the formation of copper nitrate crystals.
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3. Properties of nitric oxide and nitrogen dioxide.
a) Open the test tube (cylinder), filled with nitrous oxide and look at it against the background of
a white paper. Nitric oxide which is colorless when it comes in contact with the oxygen in the air
turns into yellow to brown nitrogen dioxide. Write the equation for this reaction.
b) When the darkening of the gas in the test tube has ended, then pour some water into it. Shake
the sample. Note the disappearance of the brown color of the gas. Test the tested solution with a
blue litmus paper. Write the reaction equation.
4. Obtaining nitrogen oxides from ammonia oxidation.
Build the device according to fig.71. Pour 2-3 ml of ammonia solution (or slaked lime mixture)
into test tube a, while pour a little mixture of Bertole's salt and manganese dioxide into test tube b.
Inside the sides and bottom of the test tube put a copper mesh or a dense layer of fine threads (this
can be made from a multi-strand conductor wire, after removing the insulating layer), and then
insert into it the tube through which you will to come the mixture of gases.
Crimp a strand of copper wire. Then heat the mixture of KClO3 with MnO2 and when the oxygen
begins to be released (test with the lit birch in the mouth of the test tube b) heat the test tube a little
with the ammonia solution. Ammonia coming into test tube c is oxidized once to NO and since
this reaction is exothermic, the strands of the copper wire are reddened. For this reason, their
(threads) heating can be interrupted.
The nitric oxide formed is easily oxidized to nitrogen dioxide with excess oxygen, which is why
the test tube gas turns yellow to brown. If the test tube is heated too much, then excess ammonia
is obtained, and as a product instead of nitrogen dioxide, a white layer of ammonium salts appears
on the sides of the test tube.
If the mixture of NH3 and O2 fails to interact on the copper wires in test tube c, then a crack inside
the apparatus may occur. Write the equation for all the reactions that occur.
5. Dimerization of nitrogen dioxide
Set up the apparatus of two small vessels joined together by a glass tube in the form of an inverted
U; on both ends of it is placed by a rubber stopper. Fill the pots and funnel with nitrogen dioxide,
prepared by the action of concentrated nitric acid on copper shavings. After filling with nitrogen
dioxide and attaching them to the side of the U-shaped funnel, immerse one of the jars in a beaker
of cooling mixture (ice and table salt), while the other jar is immersed in a beaker of warm water.
In the pot that cools, the brown to reddish color of NO2 will become weaker, due to its dimerization
in nitrogen tetraoxide (N2O4), while in the pot that heats up, the color not only remains the same,
but also intensifies.
If you change the places of the pots, then their colors will also change. The brown to weak red
color will strengthen, while the stronger one will weaken. Write the equilibrium equation for the
presence of these two nitrogen oxides.
6. Formation and decomposition of nitric acid.
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In a test tube cooled with snow or ice 2-3ml of sodium nitrite solution and then add diluted H2SO4.
Note the bluish color of the liquid due to the formation of N2O3 with the appearance of yellow-
brown NO2 gas above the liquid as a product of the partial decomposition of N2O3; Write the
equations of the reactions.
7. Oxido-reduction properties of nitrous acid.
a) Pour 2-3 ml into a test tube. acidified KI solution with dilute H2SO4 and then add a little NaNO2
solution. Note the release of free iodine which you can dictate by starch cough. Write the reaction
equation.
b) In the KMnO4 solution acidified with dilute sulfuric acid, add NaNO2 solution. Note the
discoloration of the permanganate solution as a result of the conversion of the MnOz ion to the
Mn2+ ion. Write the reaction equation.
8. Preparation of nitric acid
Build the device according to fig.72. Pour 15-20 grams of sodium nitrate into the lick and with the
side of the funnel placed inside the mouth pour some concentrated sulfuric acid so that it covers
the salt. Close the hole with a glass stopper or an asbestos-wrapped rubber stopper. Insert the neck
of the lick into a dry pot placed in a crystallizer of cold water. Heat the mixture carefully.
When a few milliliters of acid (with a weak yellow color, due to partial decomposition) have been
collected in the pot, stop the heating. Let the device cool down and then disassemble it. Save the
obtained acid for future experiments.
Be careful not to get nitric acid on your clothes or skin. It quickly destroys fabrics, while it leaves
a yellow stain on the skin and causes burns.
Write the reaction equation. Explain why crystalline NaNO3 and concentrated H2SO4 are obtained
and not solutions of these substances. Why is the reaction done by heating?
9. Decomposition of nitric acid by heating.
(do this work in the gas closet)
Pour 1-2ml into a test tube. nitric acid obtained in the previous experiment and fix it vertically on
the tripod. Heat the acid a little. Insert a lighted wooden stick held with forceps into the test tube.
Note the more energetic burning of the birch. Write the equation for the decomposition reaction of
HNO3.
10. Oxidizing properties of nitric acid.
(Perform experiments (b), (c), (d), and (e) in the fume cupboard.
a) Pour a few drops of concentrated nitric acid and a small amount of litmus or fuchsin solution
into a test tube. After mixing, the solution loses its color. Explain this change.
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b) Pour some concentrated HNO3 and a piece of sulfur into a porcelain beaker. Learn the meaning.
Sulfur is slowly oxidized to sulfuric acid. After cooling the liquid, pour some water and test for
the presence of sulfuric acid. Write the equation for the oxidation reaction of sulfur.
c) Heat some dilute HNO3 in a test tube and then bubble through it a stream of hydrogen sulphide
gas from Kipp's apparatus. Note the precipitation of free sulfur and the evolution of gas (which ?).
b) Pour 1-2 ml of concentrated HCI and a few drops of concentrated HNO3 into a test tube. Note
the chlorine output. Write the reaction equation.
e) Pour some iodine crystals and 6-8 ml of concentrated HNO3 into a small beaker. Heat the pot
until the reaction is over. Note the emission of brown to red vapors. Test for the presence of iodic
acid in the digest. Write the reaction equation.
11. Decomposition of organic substances by means of nitric acid.
Drop a drop of concentrated nitric acid on a piece of woolen cloth with the side of a glass rod. Wet
wool quickly turns yellow and then destroys.
12. Action of nitric acid on metals.
a) Pour a grain of zinc into one test tube, and a grain of tin into another test tube. Pour into both
test tubes concentrated HNO3. What gas is released?
Write the equations for the reactions assuming that zinc is converted to Zn(NO3)2 and tin to
H2SnO3.
What products are formed by the interaction of copper with diluted HNO3? Write the reaction
equation.
b) Put a grain of zinc in one test tube, while in a second one put a grain of tin, in both test tubes
put very dilute nitric acid. Shake the liquid for a few minutes, then separate the solution from the
unreacted metal. Test for the presence of NH4+ ion in the solution. Write the reaction equations,
bearing in mind that in addition to NH4NO3, nitrates of the corresponding metals are also obtained:
c) Put a little solution of 2 normal hydrochloric acid in a test tube and immerse a piece of aluminum
in it. After you see the release of hydrogen from the acids, take out the piece of aluminum, rinse it
with water and after drying it with filter paper, immerse it for a short time in fuming nitric acid.
After 1-2 minutes, carefully take out the aluminum and after rinsing it with water, immerse it again
in the hydrochloric acid. Hydrogen is no longer released. Explain the reason? Write the reaction
equation.
13. Decomposition of nitrates during heating
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a) Heat 2-3 grams of KNO3 in a test tube fixed on a tripod until the gas escapes. Test the released
gas with a lighted wooden stick. After the test tube has cooled, dissolve its contents with a little
water and test the obtained solution to see if it contains nitrites (salts of nitrous acid) based on the
reaction with Kl or KMnO4 (see experiment No. 7). Write the equation for the thermal
decomposition reaction of KNO3.
b) Do the experiment in the gas cupboard. Pour some crystals of Cu(NO3)2 into a test tube. 3H2O.
Fix the sample horizontally on the tripod and heat it very much. The salt will first dissolve in the
water of crystallization, then you will lose water of crystallization and if you continue to heat it
will decompose. Nitrogen dioxide (color) and oxygen are released. Black oxide of copper remains
in the test tube. Write the reaction equation.
Phosphorus
Phosphorus is an element that belongs to the azo group. Since the radius of its atom is greater than
that of the nitrogen atom, it attracts (up to 3) electrons weaker than nitrogen and releases them up
to 5) more easily. Phosphorus in its composition exhibits negative valence ( 3), while the positive
ones (3 and 5).
Phosphorus is known in several allotropic forms, of which white and red are of practical
importance.
Pure white phosphorus is a colorless substance with a specific gravity of 1.83 mg, a melting point
of 44C and a boiling point of 280℃. It is not soluble in water, but very soluble in many organic
solvents, for example in carbon sulfide.
White phosphorus is very poisonous and very dangerous from a fire point of view.
It combines with oxygen even at room temperature. This reaction is accompanied by a light, which
is extinguished in the dark. Finely crushed white phosphorus ignites quickly and spontaneously in
air. To protect against oxidation, it is kept under water.
When heated in the absence of air; at 250-300°C, white phosphorus is converted to red phosphorus.
Red phosphorus is a solid substance in powder form with a dark red color and a specific gravity
of 2.2. Unlike white phosphorus, red phosphorus is not poisonous, does not dissolve in carbon
sulfide and is stable in air (does not ignite by itself). During heating, it sublimates. Its vapors
condensing form white phosphorus.
These two allotropic forms have different chemical activity. White phosphorus is more active than
red phosphorus.
Phosphorus binds directly to many substances (with oxygen, halogens, sulfur and many metals),
releasing a large amount of heat. At high temperatures it also works with platinum.
Of the phosphorus oxides, phosphoric anhydride P2Os is the most important. It is formed during
the combustion of phosphorus in oxygen and is a snow-white substance that melts at 563℃.
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During the reaction, these acids with different compositions are formed: metaphosphoric acid
HPO3, pyrophosphoric acid H4P2O7 and orthophosphoric acid H3PO4.
The dissolution of P2Os in water under ordinary conditions forms metaphosphoric acid, which is
a solid substance. It dissolves well in water and is very poisonous.
Pyrophosphoric acid is a soft, glassy substance that very soluble in water. This is produced when
heating phosphoric acid to a temperature higher than 210℃.
Orthophosphoric acid (commonly called phosphoric acid) is a colorless, crystalline substance that
melts in air and is non-toxic. It is a trebasic acid and of medium strength. It forms acid salts e.g.
sodium dihydrogenphosphate NaH2PO4, sodium monohydrogenphosphate Na2HPO4 and normal
salts, e.g. normal sodium phosphate Na3PO4 called phosphates. All dihydrogen phosphates
dissolve well in water, while hydrogen phosphates and normal phosphates are soluble only salts
of alkali metals and ammonium.
Phosphoric acid is formed by boiling an aqueous solution of metaphosphoric acid in the presence
of a strong acid. Phosphoric acid is also produced during the oxidation of red phosphorus with
nitric acid as well as during the action of sulfuric acid on phosphates.
Apparatus and containers: 1) technical-chemical scale with weighing box; 2) tripod with rings
and clips; 3) lamps; 4) porcelain mortar; 5) porcelain bowl; 6) pot with porcelain lid; 7) chemical
beaker with 10 ml pupil; 8) tweezers; 11) knife; 12) tweezers; 13) asbestos mesh; 14) glass birch;
15) funnel with filter layer; 16) platinum wire.
Reagents and materials: 1) phosphorus (white and red); 2) manganese dioxide MnO2; 3) bone
ash (or phosphorus); 4) carbon sulfide CS2; 5) iron plate; 6) sheet metal; 7) litmus paper; 8) filter
paper; 9) cotton; 10) sodium hydrogen phosphate.
Solutions: 1) nitric acid HNO3 (concentrated and 2 normal); 2) sulfuric acid H2SO4 (1:1); 3)
hydrochloric acid HCl (concentrated); acetic acid CH3COOH (2 normal); 5) orthophosphoric acid
H3PO4 (1 normal); 6) ammonium molybdate(NH4)2 MoO4(2%); 7) calcium chloride CaCl2(1
normal);'8) sodium metaphosphate NaPO3 (1 normal); 9) sodium pyrophosphate Na4P2O7(1
normal); 10) normal sodium phosphate Na3PO4 (1 normal); 11) sodium dihydrogen phosphate
NaH2PO4 (1 normal); 13) sodium carbonate Na2CO3 (2 normal); 14) silver nitrate AgNO3 (O.1
normal); 15) egg white; 16) magnesium sulfate MgSO4 (1 normal); 17) a sodium hydrogen
phosphate (1 normal).
Practical work
Rules for working with white phosphorus
White phosphorus is a poisonous substance and very dangerous from the point of view of fire
(ignites at 40°C) and causes harmful burns, which are very difficult to heal. When using it, you
must take the following precautions:
1) Keep it under water
2) do not touch it with your hands, take it with tweezers or tweezers;
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3) cut in thick-walled containers (e.g. porcelain bowls) under water at a temperature lower than
26-30°C. If you use warm water for cutting phosphorus, then before doing the experiment you
should put it in cold water:
4) Dry it as soon as possible, especially if the environment is warm, by placing filter paper behind
the phosphor pieces (do not rub).
5) do not throw phosphorus on the floor, look for the fallen piece
immediately.
6) collect the small waste in water, filter it and burn it together with the wet filter on the asbestos
net in the gas cabinet.
7) If the phosphorus catches fire on your hand or body, extinguish it by covering that part of the
body with a towel. Then immediately rinse the burned area thoroughly with a 10% solution of
AgNO3 or KMnO4 and only after that make an ordinary bandage with gauze. When the burns are
serious, then after giving first aid, you should seek the help of a doctor.
1. Sublimation of red phosphorus (do this work in the gas closet)
Pour a small amount of red phosphorus into a dry test tube and close its mouth with cotton. Then
fix the test tube horizontally on the tripod and heat it gently in the weak flame of the lamp. The
red phosphorus evaporates and white phosphorus accumulates on the parts of the test tube. Be very
careful that the phosphorus vapors do not ignite as they exit the test tube.
2. Solubility of phosphorus in carbon sulfiden (Do this work away from the fire in the gas
cupboard)
a) Place in a dry test tube a small piece of white phosphorus, the size of a grain of wheat, after
having previously dried it with filter paper. Also pour 1-2 ml of carbon sulfide into the test tube.
By shaking the test tube, observe the rapid dissolution of phosphorus. Close the sample with a
stopper
and save the obtained solution for experiment 4. (Do not leave it for too long time!).
b) Test the solubility of red phosphorus in carbon sulfide in the same way.
3. Comparison of the ignition of white phosphorus and red phosphorus.
Fix an iron plate horizontally to the tripod clamp. In the middle of the plate put some red
phosphorus and closer to the clamp put a piece of white phosphorus previously dried with filter
paper. Heat the edge of the plate furthest from the clamp. You will notice that the white phosphor
will light up faster.
4. Self-ignition of phosphorus
Do this work in the gas and fireproof cabinet)
Place a piece of filter paper on a sheet of tin foil. Moisten the paper with the solution of phosphorus
in carbon sulfide prepared in experiment 2. Then take the wet paper with pliers and hold it in the
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air for a few minutes, shaking it a little. As soon as the carbon sulphide has evaporated, the finely
divided phosphorus, which remains on the paper, ignites and burns with the paper with a green
flame.
5. Reactions on phosphoric acid ions
a) Add the silver nitrate solution to the sodium hydrogen phosphate solution. Note the formation
of a yellow precipitate of Ag3PO4. Then add nitric acid. The precipitate will dissolve. Write the
equations of the reactions.
b) Add a few drops of phosphoric acid solution or normal (soluble) ammonium phosphate acidified
with nitric acid. Heat the mixture. Note the separation of the yellow crystalline precipitate of hexa-
dymolybdate of acid ammonium phosphorus.
This reaction takes place according to this equation:
H3PO4+12(NH4)2 MoO4+21HNO3=(NH4)3H4 [P(Mo2O7)6] + 21 NH4NO3 +10H2O
c) Pour a little solution of MgSO4 and NH4Cl into the solution of Na2HPO4. Add aqueous
ammonia solution to the solution mixture until the ambient reaction becomes basic. By stirring the
solution note carefully the formation of a white crystalline precipitate of MgNH4PO4. If the
precipitate is not crystalline, but in the form of hairs, then it should be dissolved with HCl or
H2SO4. Dilute the solution 2-3 times and again neutralize (neutralize) until the basic reaction with
ammonia solution. Write the reaction equation.
b) Filter the crystalline precipitate of MgNH4POc, obtained from the above test, on a quantitative
filter paper. After rinsing with dilute ammonia solution, burn the precipitate together with the filter
paper and lime it in a porcelain pot. Note the white powder of magnesium pyrophosphate
Mg2P2O7. Write the equation for the decomposition (calcification) reaction.
e) Add AgNO3 solution to the solutions of NaPO3 and Na4P2O7 found in separate test tubes.
White precipitates of AgPO3 and Ag4P2O7 are formed in both test tubes. Test their solubility in
dilute nitric acid. Write the equations of the reactions.
f) Pour some albumin solution in water into two test tubes. Pour sodium metaphosphate into one
test tube, and sodium hydnipyrophosphate into the other. Then add acetic acid to both test tubes.
In the first tube containing the mixture of sodium metaphosphate and acetic acid, observe the
coagulation of the albumin.
Based on the experiments done, draw a conclusion on how you can distinguish phosphoric acids
from one another. In which environment are silver phosphate salts precipitated?
g) Heat for 5-7 minutes a small amount of NaH2PO4 in the lid of a porcelain pot. After cooling
the obtained salt residue, dissolve it in 4-5 ml of distilled water. Test for the presence of sodium
metaphosphate solution. Write the reaction equation.
6. Phosphoric anhydride and its properties.
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(Do this work in the gas cupboard)
Pour 0.4-0.5 g. red phosphorus in a cup. At a small distance (about 0.5 cm) from the net, fix a dry
funnel. Ignite the phosphor with a heated glass rod. Phosphoric anhydride, which is formed during
the burning of phosphorus, will accumulate on the inner sides of the funnel, in the form of a white
crystalline mass that resembles snow. Write the reaction equation.
When all the phosphorus has burned, then place the funnel inside the tripod ring. Put a test tube
under the funnel and leave it like that for some time. Phosphoric anhydride will melt and liquefy
very quickly. What property does this show?
7. Preparation of phosphoric acids
a) Rinse the phosphoric anhydride, obtained in the previous experiment, with distilled water from
the sides of the funnel. Collect the rinse water in a test tube. When the solution becomes clear, then
take some of this solution in another test tube and add excess AgNO3 solution to it. A white
precipitate of AgPO3 is formed; Write the equations of the reactions.
b) Pour the rest of the HPO3 solution into a glass, dilute it with 10-15 ml of water and then add 1-
2 ml of concentrated HNO3 (to speed up the coupling reaction). Mix the contents of the glass for
5-10 minutes. Take some of the glass solution in a test tube, neutralize (neutralize) with soda until
weak acid reaction (put a piece of litmus paper in the test tube) and then add the AgNO3 precipitate.
If the coupling reaction is completed, then a yellow precipitate is formed (what is its
composition?). In the opposite case that no precipitate is formed, continue boiling for 5-10 minutes.
Again take some digest and proceed as indicated above. Write the equations of the reactions.
Lab 13-SULFUR GAS, SULFURIC ACID AND SULFATES, THIOSULFATES,
PERSULFATES.
Sulfur and hydric sulphide gas
Sulfur, like oxygen, is a typical element of group VI A of the periodic system. Its atom contains 6
electrons in its outer shell. It readily attracts two electrons but can also release up to 6 electrons.
Sulfur in its compounds has a negative valence equal to 2, while the positive valence can be 2, 4
or 6. Free sulfur is known in several allotropic forms, of which the most studied are the rhombic
forms and the monoclinic.
Natural sulfur is a yellow crystalline substance. This sulfur has crystals built according to the
rhombic system. It has a specific gravity of 2.07 and melts at 112.8°C. It crystallizes in this form
even when extracted from its solutions in carbon sulphide.
During the slow cooling of molten sulfur, needle-shaped, almost colorless crystals belonging to
the monoclinic system are formed. These have a specific gravity of 1.96 and melt at 119°C. At the
temperature below 96℃, the monoclinic form gradually changes to the rhombic one.
Sulfur is practically insoluble in water, it is slightly soluble in ethyl alcohol and benzene, but it is
especially soluble in carbon sulfide.
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The molecular mass of sulfur in solution corresponds to the formula S8 which has a cyclic
structure. During the heating of liquid sulfur to the boiling point, there are changes in its color (it
becomes darker) and mist (viscosity) that first increases and then decreases.
These changes in physical properties are caused by the opening of cyclic molecules (S8), which
have a light-yellow color, and the formation of string-type molecules, which have a red color, with
a much larger number of atoms. The entanglement (mplexia) of these sulfur macromolecules
explains the growth of its mistletoe. With the further increase in temperature, the chain
macromolecules are split and thus the mistletoe is reduced. As a result of the increase in the ratio
of chain molecules to cyclic ones, with the increase in temperature, the change in the color of
molten sulfur from yellow to red is also explained. During the rapid cooling of molten sulfur and
heated to boiling temperature, a soft mass is formed, like rubber that it is called plastic sulphur.
This turns into rhombic sulfur over time. Sulfur vapor on cooling quickly passes directly into the
solid state, forming a light-yellow powder called sulfur flower.
From the point of view of chemical properties, sulfur is an active metalloid and is quite similar to
oxygen. Like the latter, sulfur readily combines with all metals and metalloids.
It binds to hydrogen only at high temperatures, forming hydrogen sulfide H2S, or as it is called
hydrogen sulfide gas.
Hydrogen sulfide (hydrogen sulfide gas) is a colorless, rotten-egg-smelling gas, heavier than air
and highly poisonous. It is relatively soluble in water. Under normal conditions one volume of
water dissolves about 3 volumes of hydrogen sulphide gas. The aqueous solution of H2S is called
hydrogen sulfide. The latter has the property of a weak acid. As a dibasic acid, H2S forms normal
salts (sulphide) and acid salts (hydrogen sulphide). Sulfides, with the exception of (NH4)2S, Na2S,
K2S and some others, are not soluble in water.
In air, hydrogen sulphide gas burns forming sulphurous gas and water. Mixing H2S with air causes
detonation (explosion). In solution, hydrogen sulphide gas is slowly oxidized by the oxygen of the
air to free sulphur. This is a very strong reducer. It easily reduces many substances, for example,
it converts free halogens into hydrohalic acids.
Hydrogen sulfide gas is usually prepared in laboratories by the action of hydrochloric or sulfuric
acid on iron sulfide (or on sulfides of other metals).
Apparatus and containers: 1) technical-chemical scale with weight box; 2) the device according
to figure 52. 3) tripod with ring and clip; 4) lamp; 5) porcelain mortar; 6) porcelain pot with lid;
7) container with pupil 100 ml; chemical glasses with heat 250 ml 2 pieces; 9) test tube holders;
10) watch glass; 11) pliers; 12) asbestos nets; 13) glass pipes; 14) test tubes.
Reagents and materials: 1) copper (plates); 2) sulfur (sulfur cane and flowers; 3) iron sulfide
FeS; 4) carbon sulfide CS2; 5) litmus paper; 6) filter paper; 7) rubber hoses; 8) birch wood; 9)
sodium sulfate NazSO4; 10) charcoal.
Solutions: 1) sulfuric acid H2SO4 (concentrated, 1:5 and 2 normal); 2) hydrochloric acid HCl (1:1
and 2 normal); 3) ammonium sulfide (NH4)2S; 4) cadmium chloride CdCl2 (0.5 normal); 5)
potassium permanganate KMnO4 (0.1 normal), 6) potassium dichromate K2Cr2O7 (0.5 normal)
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manganese chloride or sulfate (2 normal); lead nitrate Pb(NO3)2(0.5 normal); 9) zinc sulfate
ZnSO4 (0.5 normal); 10) bromine water; 11) hydrogen sulfide water, 12) nitric acid HNO3
(concentrated).
Practical work
1. Sulfur melting
Half-fill a test tube with reeds or flowers of sulfur, which you fix on a stand inside the fume
cupboard. Heat the mixture carefully. The sulfur will begin to melt (about 113°C), forming a runny
yellow liquid. Above 160°C the liquid darkens and at 200°C it takes on a dark purple color and
becomes so misty (viscous) that it does not pour from the test tube. Above 250℃ mistletoe
decreases again and at 400℃ the sulfur turns into a free-flowing, dark brown liquid. At a
temperature of 444.5°C, molten sulfur boils, releasing orange-yellow vapors. Explain the changes
that occur when molten sulfur is heated.
2. Preparation plastic sulfur
Melt the sulfur in a test tube (see experiment 1) and pour the boiling portion as a thin stream into
a beaker of cold water. If the sulfur catches fire after pouring, then you should cover the mouth of
the test tube with a pot lid or a piece of asbestos sheet. Remove the mass of sulfur from the water
and test its elasticity by hand pulling. Save the plastic mass of sulfur formed to follow (see) the
transition from the amorphous form to the crystalline form.
3. Preparation of rhombic sulfur.
In a test tube, pour 2-3 pieces of sulfur cane, the size of a pea, and then add 10 ml. carbon sulfide.
Shaking the test tube will dissolve the sulfur. Carbon sulphide is a very poisonous liquid that burns
very easily, so do all work with it away from fire and in a fume hood. Pour a few drops of the
obtained solution on a watch glass. Set the watch glass aside until the carbon disulfide evaporates
and then observe the formation of rhombic sulfur crystals.
4. Preparation of monoclinic sulfur
Fill a porcelain pot almost full of sulphur. Place the pot on the ring of a tripod and heat it at first
with a weak flame. When all the sulfur has melted, stop heating and let the pot cool down more
slowly. Note carefully the surface of the sulfur that cools. When crystals begin to form near the
cheeks, then pour the sulfur that has not managed to freeze into a glass of water. Look at the
monoclinic sulfur crystals formed across the sides of the porcelain pot.
5. Union of sulfur with metals
Heat to boiling point a small amount of sulfur in a test tube fixed on a tripod. Then, with the help
of tongs, insert a pre-heated copper strip (narrow sheet) into the sulfur vapor. Note the vigorous
burning of copper and the formation of CuS. Write the equation for this reaction.
In a test tube, pour 2-3 pieces of sulfur cane, the size of a pea, and then add 10 ml. carbon sulfide.
Shaking the test tube will dissolve the sulfur. Carbon sulphide is a very poisonous liquid that burns
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very easily, so do all work with it away from fire and in a fume hood. Pour a few drops of the
obtained solution on a watch glass. Set the watch glass aside until the carbon disulfide evaporates
and then observe the formation of rhombic sulfur crystals.
6. Preparation and properties of hydrogen sulphide gas
Hydrogen sulphide gas is very poisonous, so do all work with it in a fume cupboard.
a) Lift the apparatus according to figure 52. Place a few pieces of iron sulfide in the test tube and
pour 3-5 ml of hydrochloric acid solution (1:1) or sulfuric acid (1:5) into it. Note the evolution of
hydrogen sulfide gas. Write the reaction equation.
b) Moisten a strip of filter paper with the lead nitrate solution and bring it close to the gas outlet
nozzle hole. Note the browning of the paper, moistened with the lead nitrate solution. Write the
reaction equation.
c) When the energetic release of gas begins, then ignite it near the gas outlet nozzle hole. Note the
combustion of hydrogen sulphide gas with a blue flame.
b) Hold a cold, dry beaker over the hydrogen sulfide gas flame. Note the formation of small water
droplets.
e) Hold a blue litmus paper moistened with water over the hydrogen sulphide gas flame. Notice its
color change. Carefully smell the combustion product. Write the equation for the combustion
reaction of hydrogen sulfide gas.
f) Cut the hydrogen sulphide gas flame with the cold lid of a porcelain pot and observe how a
yellow layer of sulfur forms on it. Write the reaction equation for the incomplete combustion of
hydrogen sulfide gas.
7. Preparation of hydrogen sulfide gas from sodium sulfate
In a porcelain mortar, powder and mix well 3g of sodium sulfate with one gram of charcoal. Pour
the resulting mixture into a porcelain pot. After closing the pot with a lid, heat it for 20-25 minutes.
After cooling, wet the contents of the pot with diluted hydrochloric or sulfuric acid. Prove that the
gas released is hydrogen sulphide. Write the equations of the reactions.
8. Solubility of hydrogen sulphide gas in water
Connect the tube of the apparatus with a rubber tube that ends with a small piece of glass tube.
Immerse the latter in the water of a test-tube or other container and bubble for a few minutes a
current of hydrogen sulphide gas. Determine the reaction (pH) of the water: hydrogen sulphide
obtained by means of tracer paper. Save this solution for the next experiment.
9. Precipitation of metal sulfides
Pour the solutions of sodium, zinc, manganese, cadmium and copper salts into separate test tubes.
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In all test tubes approximately the same amount of ammonium sulphide solution. Note the
separation and color of the ZnS (white), MnS (flesh-colored), CdS (yellow), and CuS (black)
precipitates. Write the equations of these reactions in ionic form.
Separate the obtained metal sulfide precipitates from the solutions by decantation.
Pour 1/4 of the test tube with 2 normal hydrochloric acid into each precipitate. Note which of the
precipitates dissolves in dilute hydrochloric acid. Write the equations of the reactions. Explain the
changes observed, given the solubility product of these sulphides.
Sulfur gas and sulfuric acid
Of the sulfur oxides, the dioxide SO2 (sulfuric anhydride or sulfur gas) and its trioxide SO3
(sulfuric anhydride) are the most important. Sulfur dioxide is a colorless gas with a characteristic
strong smell, poisonous and is 2.97 times heavier than air. It cools down to -10℃ and turns into a
liquid, while at -72.70℃ it solidifies into a white crystalline mass.
Sulfur gas is quite soluble in water (in 1 volume of water, under normal conditions, about 40
volumes of SO2 dissolve). During digestion, it partially reacts with water, forming sulfuric acid
H2SO3. The latter is an acid of medium strength, but unstable. It easily decomposes into SO2 and
water. Therefore, the following balances are established in the aqueous solution of sulfur gas:
SO2+H2O=H2SO3
Anhydrous (without water) sulfuric acid is unknown. Being a dibasic acid, it forms normal salts
(sulfites) and acid salts (hydrogensulfites). The latter dissolve well in water, while most sulfites
are almost insoluble in water (of the sulfites of common metals, only Na2SO3 and K2SO3 dissolve
well).
Sulfuric acid and its salts are powerful reducing substances. In their digestion, these are oxidized
slowly by air oxygen, while by oxidizing substances, such as iodine, KMnO4, K2Cr2O7, etc. they
oxidize very quickly. As a result of oxidation, sulfuric acid or its salts (sulfates) is obtained.
But sulfuric acid and sulfur gas, as sulfur derivatives with intermediate positive valence, can
sometimes also be oxidizing substances. For example, they oxidize hydrogen sulfide gas to free
sulfur. Alkaline metals and heated magnesium burn in sulphurous gas, while this does not help the
burning of a wooden birch (pine).
Sulfuric acid and its anhydride readily combine with many organic dyes, forming colorless
compounds. The bleaching process with sulfur gas is based on this property. The resulting
colorless products are decomposed by light or better by heating. Sulfur gas can be produced during
the burning of sulfur or pyrite. In the laboratory this is usually prepared by the action of
concentrated sulfuric acid on sulfites or by heating concentrated H2SO4 with copper.
Apparatus and utensils: 1) apparatus according to fig. 62; 2) tripod with clips; 3) lamp; 4)
chemical glasses with pupils 100 ml and 200 ml; 5) 100 ml student container; 6) cylinder; 7) glass
tubes that melt with difficulty (refractory) with a sphere in the middle; 8) glass tub; 9) large test
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tubes with 2 piece caps; 10) U-shaped pipe and two plugs with pipes inside (see fig. 64); 11) test
tube holder; 12) pliers; 13) spoon; 14) glass plates; 15) test.
Reagents and materials: 1) magnesium (strip and powder); 2) pyrite FeS2; 3) sodium sulfite
Na2SO3; 4) table salt NaCl; 5) ice or snow; 6) litmus paper 7) cotton; 8) large cork; 9) wooden
birch.
Solutions: sulfuric acid H2SO4 (concentrated and 2 normal); sulfuric acid H2SO3 (freshly
prepared); 3) hydrochloric acid HCl (2 normal); 4) barium chloride BaCl2 (1 normal); 5) potassium
permanganate KMnO4 (0.1 normal); 6) potassium dichromate K2Cr2O7 (0.5 normal); 7) sodium
sulphite; 10) sulphidic water; 11) litmus; 12) fuchsia.
Practical work
1.-Burning the host
Place several small pieces of pyrite in the sphere of a refractory tube. Fix the latter, obliquely, on
a tripod and then heat the sphere with a lamp. Sulfur gas, which comes out at the upper end of the
funnel, can be determined by the smell and the reddening of the blue litmus paper. Write the
reaction equation given that one of the products is Fe2O3.
2. Preparation of sulphurous gas
a) Set up the apparatus according to figure 62. Pour 2-3 spoons of sodium sulfite into the pot, while
pour concentrated sulfuric acid into the separatory funnel. Drop by drop the acid into the pot.
Collect the released gas in glasses (or cylinders) and in two large test tubes, which after you fill
them with gas, close them well with corks. Cover the glasses (or cylinders) filled with SO2 with
glass plates. Then saturate 50-100 ml of water with sulfur gas. For this, immerse the free end of
the gas pipeline (outlet) in a container with water. Be careful that the water not be absorbed into
the beaker containing the mixture of Na2SO3 and H2SO4. At the end of the experiment you can
warm the mixture slightly. Save the two test tubes and beakers containing sulfur gas, as well as
the container containing the H2SO3 solution for future experiments. Write the equation of the
reaction.
b) Pour 4-5 small pieces of copper shavings and some concentrated sulfuric acid into a test tube.
Close the mouth of the sample with a rubber stopper, through which one end of the tube passes to
remove the gas. Heat the sample with a lamp or a sand bath. Note the release of sulfur gas. Write
3. Density of sulphurous gas
Fill a glass tub full with the cooling mixture consisting of two parts snow or crushed ice and one
part table salt. In this mixture put a "U" shaped funnel with thin sides. As shown in figure 64, the
"U" pipe is connected on both sides with two other pipes, one to bring in, while the other to remove
the gas, which does not densify. Prepare the SO2 gas as in experiment 2. After 10-15 minutes, a
small amount of liquid sulfur dioxide accumulates in the funnel. After removing them from the
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cooling mixture, the liquid (liquid SO2) begins to evaporate. This evaporation is strengthened if
you warm the pipe a little by hand.
Pour the liquid SO2 into a small beaker placed over a large stopper moistened with water. The
beaker will stick to the stopper as the water turns into ice due to the decrease in temperature from
the evaporation of the SO2.
4. Extinguishing the birch wood in sulphurous gas
In a test tube filled with sulphurous gas, insert a burning wooden birch. Explain why the birch
extinguishes in the atmosphere of sulphurous gas.
5. Dissolution rate of sulfuric gas in water.
Invert a stoppered test tube filled with sulfur gas into a water crystallizer and then remove the
stopper. The water begins to rise up and fills almost the entire test tube. To speed up the dissolution
of sulfur gas, shake the test tube inside the water during the experiment. Close the test tube under
water with a stopper and remove it from the crystallizer. Test the obtained solution with a blue test
paper. Note the change in the color of the test. Write the reaction equation for the interaction of
sulfur gas with water. How else can you prove that the resulting form has acidic properties? Do
the relevant experiment.
6. Reducing properties of sulfuric acid
Into four test tubes, pour: into the first bromine water, into the second iodine water, into the third
potassium permanganate solution and into the fourth potassium dichromate solution. Add a little
diluted sulfuric acid to these last two. Then pour sulfuric acid solution into all the test tubes. In the
first three test tubes the solutions turn white (lose color), while in the fourth test tube the color of
the solution changes from orange to green. Write the equation of the four reactions taking into
account that in the third and fourth test tubes one of the products of the reaction is MnSO4
(colorless dissolution) and Cr2(SO4)3 (green dissolution) respectively.
7. Oxidizing properties of sulfuric acid
Pour into a test tube the sulfuric acid solution obtained in experiment 2 and add hydrogen sulfide.
Note the appearance of free sulfur in the form of a white tube. Write the reaction equation.
8. Combustion of magnesium in sulphurous gas
Into a beaker (or a cylinder) filled with sulphurous gas, insert a lighted strip of magnesium, holding
it with forceps. Magnesium will continue to burn even in SO2 gas forming white magnesium oxide
and free sulfur. Write the reaction equation.
9. Disappearance of fuchsia color by means of sulfuric acid
Pour the diluted fuchsia solution into a test tube and add the sulfuric acid solution to it. Note the
bleaching (loss of color) of the fuchsia. Heat the resulting colorless solution. Note the display of
the previous color. Explain the changes that occur.
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10. Reaction for the detection of SO3 ion
In the fresh solution of sulfuric acid or any sulphite (its salt) pour solution of BaCl2. A white
precipitate of BaSO3 is formed. This dissolves, if you throw in pure and concentrated hydrochloric
acid. Write the equations for the reactions. Explain the dissolution of the precipitate of barium
sulphite in hydrochloric acid, using the knowledge of the solubility product.
Sulfuric acid, sulfates, thiosulfates and persulfates
Chemically pure sulfuric acid is a colorless oily liquid (specific gravity 1.838) that freezes at 10.5C
in the form of a crystalline mass and boils at 338°C. During boiling it partially decomposes into
SO3 and H2O. Commercially available concentrated acid usually contains 98% H2SO4.
During the dissolution of sulfuric acid in water, due to hydration, a large amount of heat is released.
In no case should water be added to concentrated H2SO4, as the first drops of water instantly turn
into steam and the liquid droplets jump out of the container. Sometimes this phenomenon develops
so rapidly that it takes on the character of an explosion. To dilute the sulfuric acid, it must be
poured into the water in the form of a thin stream while continuing to mix without interruption.
Concentrated sulfuric acid absorbs moisture well, so it is often used for drying gases. It can take
water elements from some organic compounds, causing their carbonization.
Sulfuric acid that falls on the skin or on clothes should be immediately rinsed with a large amount
of water, then the place where it fell is moistened with a dilute solution of ammonia and again
rinsed with water.
Concentrated sulfuric acid is a very strong oxidizing substance. During heating it oxidizes almost
all metals, reducing itself to SO2 in free sulfur or H2S depending on the activity of the metal and
the temperature. Under ordinary conditions, concentrated sulfuric acid does not act on iron. Dilute
sulfuric acid dissolves metals, which are to the left of hydrogen in the voltage range, forming the
salts of these metals and releasing hydrogen.
Concentrated sulfuric acid is a very strong oxidizing substance. During heating it oxidizes almost
all metals, reducing itself to SO2 in free sulfur or H2S depending on the activity of the metal and
the temperature. Under ordinary conditions, concentrated sulfuric acid does not act on iron. Dilute
sulfuric acid dissolves metals, which are to the left of hydrogen in the voltage range, forming the
salts of these metals and releasing hydrogen.
Sulfuric acid is a strong dibasic acid. It forms normal salts (sulfates) and acids (hydrogen sulfates).
Sulfates that have the composition MeSO4.7H2O (where Me is Fe, Zn or Ni, etc.). form a group
called vitriol. Shapes are another group of double sulfates that have the general formula
M2SO4.Me2(SO4)3 24 H2O (where M is Na+e K+or NH4+, while Me is Al3+,Cr3+ or Fe3+).
All these hydrogen sulfates and many sulfates dissolve easily in water. Of the common metal
sulfates, CaSO4 is slightly soluble, while BaSO4 and PbSO4 are practically insoluble.
During heating, some sulfates, such as CuSO4, Fe2(SO4)3, decompose into sulfuric anhydride and
metal oxide, other sulfates, such as Na2SO4, K2SO4, CaSO4, do not decompose even at 1000℃.
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By replacing an oxygen atom with a sulfur atom in sulfuric acid or its salts, they are formed,
respectively. thiosulphuric acid H2S2O3 or its salts called thiosulphates. The latter can be
produced by boiling sulphite solution with sulphur, e.g.:
During the acidification of thiosulfate solutions, very unstable thiosulfuric acid is formed, which
immediately decomposes into H2SO3 and sulfur. Only the normal salts of thiosulfuric acid are
known. Most of these dissolve well in water. Some of them easily form supersaturated solutions.
The Na2S2O3 salt has the greatest practical importance. 5H2O which is sometimes erroneously
called hyposulphite.
Since there is a sulfur atom with negative valence (two) in the molecule of thiosulfates, they are
reducing substances. Under the action of strong oxidizing substances (for example chlorine)
thiosulfates are oxidized to sulfates (in sulfuric acid salts). Less powerful oxidizing agents (for
example iodine) convert these to tetrathionic acid salts H2S4O6. Based on this equation:
By replacing both hydrogens in the hydrogen peroxide molecule (H-O-O-H) with two HSO3
groups, the peroxidisulfuric or persulfuric acid molecule with the formula H2S2Os is formed. The
salts of this acid are called peroxydisulfates or persulfates and have oxidizing properties. The
oxidizing properties of the acid and persulfates are explained by the peroxide bond found in them:
Apparatus: 1) tripod with clips; 2) lamp; 3) glass tub; 4) test tube holder; 5) glass rod;
Reagents and materials: 1) iron (powder); 2) copper (particles), 3) zinc (granules); 4) sulfur
(pieces and powder); 5) coal (pieces); 6) trivalent iron sulfate Fe2(SO4)3 and divalent
FeSO4.7H2O; 7) divalent copper sulfate (cupric) CuSO4.5H2O; 8) sodium sulfate Na2SO4; 9)
thiosulfate
sodium (Na2S2O3.5H2O,0.1 N); 10) sugar Cı2H22O1ı (powder); 11) filter paper; 12) litmus
paper; 13) birch wood; 14) sodium sulfite Na2SO3.
Solutions: 1) sulfuric acid H2SO4 (concentrated and two normal); 2) hydrochloric acid HCl
(concentrated and two normal); 3) nitric acid HNO3 (concentrated); 4) barium chloride BaCl2 (1
normal); 5) lead nitrate Pb(NO3)2. 6) chlorine water; 7) iodine water; 8) starchy cough; 9)
potassium iodide K1 (0.1 normal); 10) ammonium or potassium persulfate (NH4)2S2O8 (1
normal); 11) sodium hydroxide NaOH (1 normal); 12 sodium thiosulphate Na2S2O3 (0.1)
normal).
Practical work
1) Preparation of sulfuric anhydrite by the contact method.
(Do this work in the gas cupboard)
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Fill a dry hot pot with 200-300 ml of sulphurous gas. Turn the mouth of the filled pot to the
horizontal position for a few minutes in order for some of the sulphurous gas to escape into the
atmosphere and be replaced by air, close the pot containing the gas mixture with a cork and invert
it several times, so that the mixture of gases as best as possible. Place a platinized asbestos sphere
in an iron spoon. Heat the spoon with the asbestos and then quickly put it inside the pot. Note the
formation of sulfuric anhydride vapor around the catalyst. Write the reaction equation.
2) Dilution of concentrated sulfuric acid.
Fill 1/4 of the test tube with water and carefully add 1-2 ml of concentrated sulfuric acid, shaking
the test tube constantly. Note the heating of the liquid. Explain why water should not be added to
sulfuric acid during dilution.
3) The action of taking water from the side of concentrated sulfuric acid a) Put some concentrated
sulfuric acid in a test tube and dip a wooden stick in it. Explain the cause of its carbonation.
b) Pour 5-6 grams of powdered sugar into a small chemical beaker placed inside a glass tub. At
first, add a little water to the sugar until a thick slurry is formed, then 5-6 ml of concentrated
sulfuric acid. Mix the contents of the glass well with a glass straw. Explain the cause of the
carbonation of the sugar and the lumpiness of the mass.
c) Write something with diluted sulfuric acid on a piece of paper with the help of a sharp wooden
stick. Dry the paper carefully near the flame of the lamp. Put the writings on the paper and explain
the phenomenon.
4) Oxidizing properties of concentrated sulfuric acid.
Place a small piece of sulfur in one test tube and a piece of charcoal in a second test tube. Pour a
little concentrated sulfuric acid into each test tube and heat carefully. Smell (carefully) the odor of
the gas that is formed. Write the equations for the reactions bearing in mind that sulfur is oxidized
to SO2, while carbon is oxidized to CO2 and sulfuric acid is reduced to SO2.
5) The action of sulfuric acid on metals.
(You do these tests in the gas cabinet)
a) Put some copper shavings in a test tube. Add 2-3ml of concentrated H2SO4 and heat carefully.
Carefully smell the gas that is formed. After the experiment, when the test tube has cooled down,
pour the liquid, while adding 5-6 ml of water to the remaining sawdust, then shake the test tube.
The resulting solution is colored blue by Cu2+ ions, indicating that CuSO4 is formed; Write the
equation for the reaction.
b) Place 1-2 grains of zinc in a test tube; add some concentrated H2SO4 and heat carefully. As a
result, sulphurous gas is released, which you can detect based on the smell. On further heating, the
liquid in the test tube becomes turbid due to the formation of free sulfur in a state of fine dispersion,
while the escaping gas also has the smell of hydrogen sulphide gas. Write the three reaction
equations bearing in mind that in all cases ZnSO4 is obtained and that in the first case sulfuric acid
is reduced to SO2, in the second to S and in the third to H2S.
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What property of sulfuric acid is pointed out by these experiments? Explain the difference in the
action of concentrated H2SO4 on Zn and Cu.
c) Develop in test tubes the reactions of mutual interaction of dilute sulfuric acid with zinc and
iron. Write the equations of the reactions. How does diluted H2SO4 act on copper?
6) Reaction for the detection of SO4 ion
a) Pour the barium chloride solution into a test tube and add dilute sulfuric acid or a solution of
any soluble sulfate. Note the color of the precipitate. Write the reaction equation in ionic form.
Add concentrated hydrochloric acid to the precipitate produced. Does the precipitate dissolve?
Ba2+ ion is reactive for SO42 ion
b) Pour the lead nitrate solution into a test tube and add dilute sulfuric acid or a solution of any
ternary sulfate. A white precipitate of PbSO4 will be treated. Write the reaction equation in ionic
form.
7. Concentration of sulfate salts against heating.
a) Put some pressed copper sulfate crystalline hydrate in a dry test tube. Fix the sample on the
tripod vertically in such a way that its end is higher than the nozzle. Heat the copper sulfate. Notice
how it first emits water and then turns into a black powder, copper oxide.
Insert a piece of blue litmus paper into the steam that forms. Write the equation for the
decomposition reaction of copper sulfate.
b) Do a similar experiment with iron sulfate and Glauber's salt. Do all these salts break down
during digestion to release SO3?
8) Decomposition of thiosulfuric acid
Dissolve 2-3 crystals of sodium thiosulfate in water and add small amount of 2 normal solution of
HCl. After a while you notice the blurriness. of the solution and then the formation of the
precipitate. Take note of the smell of the gas being released. How can it be proved that the
precipitate consists of free sulphur? Write the reaction equation.
9) Formation of sodium thiosulfate
Pour into a test tube some saturated solution of sodium sulphite and then add about 0.5 gram of
powdered sulphur. Heat this mixture carefully and let it boil for 10-15 minutes. Filter the solution
to separate from the sulphide excessive.
To test for the formation of sodium thiosulfate, add an excess of 2 normal HCl to a portion of the
filtrate. What will you notice? Write the equations of the reactions
10. Preparation of supersaturated solution of BaS2O3
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Dissolve sodium pectin sulfate in 3-4 ml of water and add the BaCl2 solution. You won't notice
any difference. With the side of a glass rod, rub the inside of the test tube below the level of the
liquid. Note the formation of a large amount of crystals. Write the equation for this reaction.
11. Reducing properties of sodium thiosulfate.
a) Add a drop of chlorine to the sodium thiosulfate solution. Note the disappearance of the chlorine
smell. Prove that SO42 ions are present in the solution. Write the reaction equation.
b) Add a few drops of iodine water to the sodium thiosulfate solution. The color disappears.
Explain the emerging phenomenon. Write the reaction equation.
12. Determining the normality of iodine digestion by sodium thiosulfate
Determination of the normality of iodine dissolution is based on the reaction described above (exp.
12,b). For this, accurately pour 10 or 25 ml of iodine solution into a conical flask. Using a burette,
titrate the iodine solution with 0.1 or 0.05 N sodium thiosulphate solution. In the beginning, make
the titration fast, but when the color of the iodine solution changes to light yellow (cheet); then
add 1-2 ml of starch solution and continue the titration with thiosulfate until the blue-violet color
of the conical flask solution is completely whitened.
Calculate the normality of dissolution of iodine knowing the normality of dissolution of sodium
thiosulfate.
13) Oxidizing properties of persulfates
a) Pour 3-4ml of potassium iodide solution and cerium hydrochloric acid into a test tube until it
becomes an acidic environment. Add a few drops of persulfate solution (sodium or ammonium) to
the acid solution. Note the release of free iodine. Write the reaction equation.
bj Dissolve a few recrystallized crystals of ferrous sulfate in 5-6 ml of distilled water. Divide the
obtained solution into two test tubes. In one test tube a little solution of some persulfate and then
in both test tubes pour sodium hydroxide solution. Note if the precipitates of both test tubes have
the same color. What is the reason? Write the equations of the reactions.
Lab 14-COPPER AND SILVER. ZINC, CADMIUM, MERCURY
Copper and silver
Copper, silver and air are elements of group I-B of the periodic system. Their atoms, like those of
alkaline metals, have an electron in the outer layer, so they lack the ability to attract electrons. But
unlike the alkaline metals, atoms of Cu, Ag and Au in the penultimate layer have not 8, but 18
electrons, which determines the difference in their properties. The radii of the atoms of the
elements of the copper group are much smaller than the radii of the atoms of the alkali metals that
remain in that period, therefore the last electron is held more strongly by the nuclei of Cu, Ag and
Au atoms. These elements are oxidized more difficult than the alkali metals, while their ions are
reduced more easily. Since the layer of 18 electrons near Cu, Ag and Au atoms is not completely
stable, then these can give not only the outer electron, but also a part of the electrons of this layer.
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Copper in its composition is presented as monovalent and divalent, but under normal conditions
the most stable are the compounds of divalent copper. While silver is almost always monovalent.
Copper is a yellow to red metal, silver is a white metal and gold is yellow.
From the point of view of chemical properties, bact and silver are slightly active metals. I noticed
that in the sequence of tensions these are to the right of hydrogen, they do not take this out of its
compounds and dissolve in those acids that are oxidizing. In concentrated and hot sulfuric acid
copper and silver dissolve forming the corresponding salts and SO2; in nitric acid forming salts,
NO or NO2 depending on its concentration. Copper can be produced by reduction by heating its
oxide with charcoal or in hydrogen. Copper can also be produced by electrolysis of its salts or by
displacement from other more active metals that lie in the voltage range to the left of hydrogen
(e.g. from non-existent).
Almost all copper and silver compounds are easily reduced to metals.
Copper forms the oxides Cu2O (cuprous oxide) and CuO (cupric oxide). Copper oxide Cu2O has
a red color, it is practically insoluble in water. Cupric oxide hydrate CuOH is unstable compound
and easily decomposes into cupric oxide and water.
Silver oxide Ag2O is almost insoluble in water and combines with it to a small extent to form the
hydrate AgOH, which is a fairly strong base. AgOH easily decomposes into silver oxide and water,
therefore, during the interaction of solutions of silver salts and alkalis, a dark brown precipitate of
Ag2O is formed.
Cu+ salts and most Ag' salts are insoluble in water. Of the silver salts, silver nitrate AgNO3 (lapis)
is mostly used. Under the action of light, most silver compounds break down, separating the
metallic silver. More sensitive to light are silver halides, which are widely used in photography.
Compositions of The black copper oxide CuO and its corresponding blue hydrate Cu(OH)2 are
insoluble in water, but readily dissolve in acids giving 220.
formed salts. Cu(OH)2 also partially dissolves in concentrated solution of strong alkalis forming
salts called cuprites (for example Na2CuO2).
Most divalent copper salts are soluble in water. The hydrated Cu2+ ion is blue in color. Copper
iodide Cul2 is unstable under ordinary conditions, therefore, during the interaction of dissolved
salts of Cu2+ with soluble iodides of metals, copper iodide Cul and free iodine are produced. In
aqueous solutions, copper salts undergo hydrolysis.
Copper and silver form complex compounds, which usually dissolve easily in water. For this
reason, many copper and silver compounds insoluble in water can pass into soluble complex
compounds. The coordination number of Cu+ and Ag' is usually 2, while that of Cu2+ is 4.
Appliances and containers: 1) accumulator (4-6 volts); 2) device according to fig. 79; 3) stand
with clips and rings; 4) lamp; 5) U-shaped pipe; 6) water bath; 7) funnel; 8) student glasses 100
ml-2 pieces; 9) asbestos mesh; 10) test tube holder; 11) pot with 1 liter student; 12) porcelain cup.
92
Reagents and materials: 1) copper; 2) iron (powder) or zinc; (granulated); 3) charcoal (dust); 4)
copper oxide CuO; 5) platinum or nichrome wire; 6) coal electrodes (2 pieces); 7) copper wire; 8)
litmus paper; 9) filter paper; 10) mercury (Hg).
Solutions: 1) nitric acidHNO3 (concentrated and 2 normal); 2) sulfuric acid H2SO4 (concentrated
and 2 normal); 3) hydrochloric acid HCl (concentrated and 2 normal); 4) sodium hydroxide NaOH
40% and 2 normal; 5) ammonium hydroxide NH4OH (25% and 2 Normal); 6) calcium hydroxide
Ca(OH)2 (saturated); 7) potassium iodide Kl (0.1 normal) 8) potassium bromide KBr (0.5 normal);
9) sodium chloride NaCl (2 normal); 10) sodium thiosulfate Na2S2O3 (0.1 normal); 11) sodium
carbonate Na2CO3 (2 normal); copper sulfate CuSO4(0.5 normal); 13) copper chloride CuCl2(0.5
normal); 14) silver nitrate AgNO3(0.1 normal); 15) formalin HCHO (2%) glucose
C6H12O6(10%); 17) starchy cough.
After the experiment, collect all solutions and precipitates that contain silver in a special pot that
you can use.
Practical work
1. Reduction of copper oxide by charcoal
Build the device according to fig.78. Put a small amount of the mixture prepared from equal parts
of cupric oxide and charcoal powder into the test tube. Place the end of the degassing tube in the
test tube containing the lime water and then heat the mixture strongly for a few minutes. Note the
turbidity of the lime water. After the test tube has cooled, pour its contents onto a sheet of paper.
You can detect the copper that is formed as a result of this reaction based on its color. Write the
equations of the reactions
2. Extraction of copper from its salts by means of other metals.
Pour the copper sulfate solution into a test tube and add iron powder or 1-2 grains of zinc there.
Close the container with a cork and shake carefully. Watch the color change of the solution and
the iron or zinc powder. Write the reaction equation.
Instead of the accumulator, the current of the city's lighting network can be used, transformed and
rectified. In this case, the rectifier is connected in series with the pipe.
3. Coloration of the flame by means of copper salts
Dip a piece of platinum or nichrome in concentrated hydrochloric acid and burn it in the flame of
the lamp. Then put it in the solution of some salt and again put it in the flame of the lamp. Look at
its color.
4. Copper resistance to acids
(Do this work in the gas cupboard).
Pour small amounts of copper filings into separate test tubes and add concentrated and dilute acids
HCI, H2SO4 and HNO3. Notice the phenomena that occur.
93
Atc test tubes in which the reaction does not start in the cold, heat them.
Does copper react with all acids? Write the equations of the reactions.
5. Cooking properties of copper hydroxide
Add sodium hydroxide solution to a copper salt solution. A blue gelatinous precipitate of Cu(OH)2
is formed. Write the reaction equation.
Shake the obtained precipitate, divide it into two test tubes and study its attitude against dilute
acids and against the concentrated excess of alkalis. Note the color of the solutions obtained. Write
the equations of the reactions.
6. Decomposition of copper hydroxide
Prepare copper hydroxide (see experiment 5). Heat the liquid with the precipitate until it boils. The
precipitate gradually turns black due to the formation of black copper oxide. Write the reaction
equation.
7. Hydrolysis of copper salts
a) Test the dissolution of CuSO4 with red and blue litmus paper. Explain the change that occurs
in the color of litmus paper. Write the equation for the hydrolysis reaction of CuSO4. What
conclusion can be drawn regarding the properties of copper hydroxide as a base?
b) Add the solution of Na2CO3 to the solution of CuSO4. Note the formation of a green precipitate
of basic copper carbonate and the evolution of carbon dioxide. Write the reaction equation.
8. Preparation of cuprate tetramine sulfate solution
Add the ammonia solution to the CuSO4 solution until the precipitate of the basic salt formed at
the beginning is dissolved. A blue to purple solution is formed. Write the reaction equation. In the
composition of which ion is copper a part? What is the color of this ion? This reaction is often
used to detect Cu2+ ions;
9. Preparation of copper oxide and its hydrate
Add 1-2 ml of the CuSO4 solution to the excess sodium hydroxide solution and the glucose
solution. In the beginning, a yellow-orange precipitate is formed, which upon stronger heating
gradually transforms into the red copper oxide Cu2O.
2Cu(OH)2+C6H12O6=Cu2O+C6H12O7+2H2O.
What properties does copper hydroxide present in this reaction?
10. The benefit of copper iodide
Add the KI solution to the CuSO4 solution. Allow the precipitate of copper iodide (CuI ) to
separate at the bottom. Decant a part of the solution, dilute it with water and add a little cornstarch.
94
The digestion takes on a blue color. What substances are produced by the interaction of CuSO4
with KI? Write the reaction equation.
To convert free iodine into a colorless compound, add sodium thiosulphate or sulfuric acid solution
to the test tube containing the precipitate until the brown color disappears. White copper iodide
remains at the bottom of the test tube. Write the reaction equation.
11. Extraction of silver from its salts with other metals
Pour 2 ml (approx) of AgNO3 into two separate test tubes. Insert a copper wire into one test tube,
and drop a drop of mercury into the other test tube. Note the slow separation of metallic silver and
write the reaction equations.
12. Preparation of the silver mirror.
Pour the 10% solution of AgNO3 into a well-washed test tube and add the ammonia solution drop
by drop until the precipitate formed at the beginning is dissolved. Then add a 10% glucose or
formalin solution. Heat this mixture in a water bath. After a few minutes the inner surface of the
test tube is coated with a shiny metallic silver coating.
13. Formation of silver oxide and metallic silver
Add the sodium hydroxide solution to the silver nitrate solution. Note the formation of brown
precipitate of silver oxide. Heat the contents of the test tube to boiling, filter it, rinse the solid mass
(Ag2O) with water on the filter paper and then place the latter together with the contents in a
porcelain bowl. Place the container with the contents to dry and then burn the paper and calcine
its contents. Note the metallic silver coming out. Write the reaction equation.
14. AgNO3 dissolution reaction with litmus
Test the dissolution of AgNO3 with red and blue litmus paper. What is the digestion reaction?
What can you conclude about the properties of silver hydroxide as a base?
15. Silver halides
a) Pour the AgNO3 solution into three test tubes and add the NaCl solution to one of them, the
KBr solution to the other and the KI solution to the last one. In the first test tube, a white precipitate
of AgCl is formed, in the second a lemon yellow precipitate of AgBr, and in the third a yellow
precipitate of AgI. Write the equations of the reactions.
b) Filter the obtained precipitate of AgCl and let it stand in the light (it is better to stand in direct
sunlight). Due to the separation of silver, the precipitate gradually darkens, then it becomes purple
and more black skirt. Write the reaction equation.
Zinc and cadmium
Zinc, cadmium and mercury form group II B of the periodic system. Their atoms, as well as all
elements of this group in the outer layer, have 2 electrons, Zn, Cd and Hg in the penultimate layers
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contain 18, and not 8 electrons, like magnesium and other alkaline earth metals. This explains
exactly the difference in the properties of the elements of group II A (Mg-Ba) and group II B (Zn-
Hg). Zinc, cadmium and mercury are less active reducing agents and tend to form complex
compounds.
Zinc and cadmium release two electrons quite easily, therefore in their compounds they are always
positively divalent. These are metals with white like silver, but in humid air they oxidize little by
little and their surface loses its luster.
In the range of voltages, these are to the left of hydrogen, therefore zinc in dilute acids dissolves
easily, while cadmium more slowly, taking out hydrogen. In concentrated sulfuric acid, cadmium
dissolves forming sulfate and SO2, while zinc, in addition to sulfate, also forms SO2, S, H2S. In
nitric acid, these dissolve forming the corresponding nitrates and various oxides of nitrogen or
ammonia (according to the concentration of the acid).
Zinc also dissolves in concentrated solutions of strong alkalis, giving off hydrogen and forming
salts called zincates.
This process takes place in two stages. First the alkali dissolves the protective film of zinc oxide
on the surface of the metal, then the latter with water extracting hydrogen and forming Zn(OH)2,
which also dissolves in alkali.
1) ZnO+2NaOH=Na2ZnO2+2H2O
2) Zn+2H2O=Zn(OH)2+H2
3) Zn(OH)2+2NaOH=Na2ZnO2+2H2O
The general draw of the second and third stages
Zn+2NaOH= 2ZnO2+H2
Both in the acid environment and in the alkaline one, zinc appears as a strong reducer.
Zinc and cadmium form the oxides ZnO and CdO, the hydrates of these oxides Zn(OH)2 and
Cd(OH)2 are insoluble in water, but dissolve easily in acids. Cd(OH)2 is insoluble in alkalis, while
Zn(OH)2 is an amphoteric hydroxide whose basic properties prevail over acidic ones.
Zn2+ and Cd2+ ions are colorless. Many zinc and cadmium salts are soluble in water. Among the
insoluble salts, the most characteristic are white ZnS and yellow CdS sulfides. In aqueous
solutions, soluble zinc and cadmium salts are hydrolyzed.
Zinc and cadmium have properties to form complex compounds. Thus, during the interaction of
zinc or cadmium salts with ammonia or ammonium salts, mines (ammoniacates) are formed.
Apparatus and vessels: 1) Kip's apparatus filled with FeS and acid. 2) lamp; 3) zinc; 4) test tube
holders; 5) iron spoon for burning; 6) brick or tile.
96
Reagents and materials: 1) zinc (granular and powder); 2) paper: litmus; 3) filter paper; 4)
wooden birch; 5) flower of sulfur.
Solutions: 1) nitric acid HNO3 (concentrated and 2 normal); 2) sulfuric acid H2SO4 (concentrated
and 2 normal); 3) hydrochloric acid HCl, (concentrated and 2 normal); 4) acetic acid CH3COOH
(2 normal); 5) sodium hydroxide NaOH (40% and 2 normal); 5) ammonium hydroxide NH4OH
(2 normal); 7) ammonium sulphide.(NH4)2S; 8) ammonium chloride NH4Cl (2 normal); 9)
cadmium sulfate CdSO4 (0.5 normal); 10) sodium carbonate Na2CO3(2 normal);11) sodium
acetate CH3COONa (2 normal); 12) zinc sulfate ZnSO4 (0.5 normal); 13) sulphidic water; 14)
potassium nitrate KNO3(2 normal); 15) potassium hydroxide KOH (2 normal).
Practical work
1a) Take some zinc powder in an iron spoon, which you heat in the upper part of the flame of the
gas lamp. Note the burn and color. of the product. Write the reaction equation.
b) Take a small amount of flowers of sulfur and sprinkle twice as much sulfur on it. Mix
carefully in the fume hood. Place a portion of the mixture on a brick and with the side of a long
stick light it. Note the process of combining zinc with sulphur, which is often accompanied by
strong crystals, as well as the color of the product.
2) Interaction of zinc with acids
a) Test the action of hydrochloric acid and dilute sulfuric acid on zinc grains in separate test
tubes. Write the reaction equations.
b) Test the action of concentrated hydrochloric acid on zinc. Are there differences in the action
of diluted hydrochloric acid and concentrated hydrochloric acid on zinc?
Compare the action of concentrated and dilute sulfuric acid on zinc.
d) Put a small grain of zinc in a test tube and add some dilute nitric acid. If gas formation is
observed, then dilute the solution with water. Let the contents of the test tube stand for 10-12
minutes. To prove that the products produced are ammonium salts, you must add sodium
hydroxide solution to the contents of the test tube until the alkaline reaction (litmus paper test).
Heat the sample to boiling and detect the ammonia which is formed by means of a wet piece of
red litmus paper placed in the steam. Write the equations of the reactions.
e) (Perform the experiment in the gas cupboard). Test the action of concentrated nitric acid on
zinc. What substances are obtained? Write the reaction equation.
3. Interaction of zinc with alkalis
Take some zinc dust in a test tube and add to it the concentrated solution of some strong alkali and
heat it. Note the evolution of gas and the dissolution of zinc, which forms zincate. Write the
reaction equation.
4. Preparation of zinc hydroxide
97
a) Add a little sodium hydroxide solution to the zinc sulfate solution. Note the formation of a white
gelatinous precipitate of Zn(OH)2. Write the reaction equation.
b) Divide the formed precipitate in half into two test tubes. Add dilute acid to one test tube, and
add excess sodium hydroxide to the other until the precipitate dissolves. Write the reaction
equations in molecular and ionic form. In which ions does zinc hydroxide dissociate in aqueous
solutions?
c) Prove the action of concentrated sulfuric acid on zinc. in the cold and during heating. What
substances are obtained? Write the equations.
Mercury
Mercury is an element of the zinc group. It emits its two outer electrons with more difficulty than
the other elements of this group. In mercury compounds it is positively divalent. There are also
derivatives su he is formally monovalent, These compounds are called mercury. It has been
verified that they contain Hg-Hg groups and consequently both mercury atoms are divalent.
Mercury at ordinary temperature is a liquid metal; it freezes at -39°C, boils at + 357°C and has a
specific gravity of 13.6.
Mercury with many metals readily forms alloys called amalgams. In air, under normal conditions,
it does not change, while heating it oxidizes more slowly.
Unlike zinc and cadmium, mercury does not liberate hydrogen from acids, so it does not react with
dilute acids. On heating, it dissolves readily in dilute and concentrated nitric acid as well as in
concentrated sulfuric acid.
Mercury forms two oxides; mercuric oxide or simply HgO oxide in red or yellow color and
mercuric oxide or mercuric prooxide Hg2O in black color. Hg2O is an unstable compound and
gradually decomposes into HgO and mercury. Hydroxides of the latter are not known. During the
action of alkalis on solutions of mercury and mercury salts, HgO and Hg2O are formed,
respectively. Mercuric oxide dissolves well in acids, but does not dissolve in excess of alkalis.
Most mercury salts are soluble in water. Some of these, such as mercuric chloride or HgCl2
sublime in solutions are slightly dissociated. Almost all mercury salts are insoluble in water. The
most useful ones are mercuric chloride or calomel Hg2Cl2, which is a white insoluble substance,
and Hg2(NO3)2 H2O - mercuric nitrate with colorless crystals soluble in water. Many mercury
compounds are unstable and decompose into mercury compounds and metallic mercury. Hg2+ and
Hg22+ ions are colorless. Soluble mercury salts in aqueous solution undergo hydrolysis, as a result
of which basic salts are usually formed.
Mercury compounds during mutual action with strong reducing substances are easily reduced to
metallic mercury.
Mercury compounds with some salts form complex compounds for example:
HgI2+2KI= K2[H HgI2+2KI=K2[HgI4].
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The coordination number of the Hg2+ ion is 4.
Apparatus and dishes: 1) stand with rings; 2) light bulb; 3) porcelain mortar with press; 4)
porcelain bowl; 5) test tube holder; 6) asbestos net; 7) tweezers; 8) saws.
Reagents and materials: 1) Wednesday; 2) sodium; 3) copper plate (or copper coin) 4) mercuric
nitrate Hg(NO3)2; 5) mercury nitrate Hg2(NO3)2; 6) litmus paper; 7) filter paper; 8) wooden
sticks; 9) flowers of sulfur; 10) crystalline iodine.
Solutions: 1) nitric acid HNO3 (concentrated, 1:1 and 2 normal); 2) hydrochloric acid HCl (2
normal); 3) sodium hydroxide NaOH (2 normal); 4) ammonium chloride NH4Cl (saturated); 5)
potassium iodide KI (0.1 normal); 6) tin chloride SnCl2 (0.5 normal); 7) mercury nitrate Hg(No3)2
(0.45 normal); 8) mercuric chloride HgCl2 (0.5 normal); 9) mercury nitrate Hg2(NO3)2 (0.5
normal).
Practical work
Note: Mercury vapor and all its soluble compounds are very poisonous, so special care is required
when working with mercury and its compounds.
Pour all the waste mercury and solutions of its salts into a separate container to use for mercury
extraction.
1. The extraction of mercury from its salts.
Pour diluted nitric acid into a porcelain cup and add a few pieces of copper (plates) or a copper
coin to it. When the surface of the metal is clean, pour off the acid and rinse the coin in water.
Then put it back in the porcelain cup and add to it a solution of some salt of mercury. After the
mercury is separated from the coin, take out the latter and wipe it with filter paper. Note the change
in appearance of the surface of the coin. Write the reaction equation.
2. The combination of mercury with sulfur and iodine
a) Mix a few drops of mercury with a small amount of flower of sulfur in a porcelain mortar. Note
the color of the mercury sulfide that forms.
b) (Do this experiment in the gas cupboard!). Pour a drop of mercury and a few crystals of iodine
into a dry test tube. Heat the sample slowly. On the inside of the test tube, note the color of the
mercuric iodide that forms. Write the equations of both reactions.
3. Preparation and properties of sodium amalgam
(Do the work behind the glass of the gas cabinet).
Pour a few drops of mercury into a porcelain mortar. Take a small piece of sodium metal and break
it up in a porcelain bowl into even smaller particles (about the size of a pea). Take the pieces of
sodium with pliers and after wiping them with filter paper, throw them in mercury, press them
with the mortar press. In this case, the action of sodium on mercury occurs, which is accompanied
99
by ignition. According to the amount of sodium and the temperature, the resulting amalgam can
be liquid or solid.
Pour a portion of the amalgam into a test tube with water. The more sodium the amalgam contains,
the more hydrogen will be released. Test the resulting solution with litmus paper. Write the
reaction equation. Does sodium metal greatly change its chemical property in amalgam?
4. Ammonium amalgam
During the interaction of sodium amalgam with a saturated solution of an ammonium salt, sodium
is replaced by an ammonium group. The latter in amalgam is usually stable because it decomposes
very slowly into ammonia and hydrogen.
Place a small piece of sodium amalgam obtained in the previous experiment in a test tube and add
a little saturated ammonium chloride solution to it. Ammonium amalgam will form. Due to the
release of gases during the subsequent decomposition of ammonium amalgam, it increases in
volume, becomes friable and porous. After the decomposition of the amalgam, mercury remains
in the test tube. Write the equations for the reactions accepting NaHg as the formula for sodium
amalgam.
5. Preparation of mercuric nitrate
(Do the work in the gas closet)
In a porcelain cup, heat 2-3 drops of metallic mercury with 3 ml. concentrated nitric acid. If the
mercury is not completely dissolved, then add a little more acid. Write the reaction equation.
Dilute the obtained solution with water and save it for the experiment. next.
6. Preparation of mercury oxide
To the mercuric nitrate solution obtained in experiment 4, add the sodium hydroxide solution. Note
the separation of a yellow precipitate of mercuric oxide. Write the reaction equation. Test the
stability of mercuric oxide against excess alkali and dilute acid.
7) Hydrolysis of mercury salts
In a small amount of water, dissolve a few crystals of mercuric nitrate or sulfate. Observe the
formation of the basic salt precipitate. Test the digestion reaction using litmus paper. Write the
reaction equation.
8. The action of potassium iodide on soluble mercury salts.
Add a little potassium iodide solution to the solution of any mercuric salt. Note the formation of a
red precipitate of HgI2. Write the reaction equation.
Add back an excess of potassium iodide until the red precipitate dissolves. Write the equation for
the reaction that yields the complex salt K2[Hgl4].
100
9. Reduction of mercury salts
Add a little of the stannous chloride (divalent tin) solution to the sublime solution. Note the
formation of a white precipitate of calomel. Write the reaction equation. Then again add an excess
of the stannous chloride solution, and the precipitate will take on an ash color, owing to the escape
of metallic mercury. Write the reaction equation.
10. Preparation of mercury nitrate
(Do the work in the gas closet)
In a porcelain cup, heat 2-3 drops of metallic mercury together with 1-2 ml of diluted nitric acid
(1:1). Part of the mercury in this case will remain undissolved. After completion of the reaction,
dilute the solution and save for future experimentation.
11. Preparation of mercury oxide
Add the sodium hydroxide solution to the mercuric nitrate solution. Note the formation of a black
precipitate of mercuric oxide. Write the reaction equation.
12. Hydrolysis of mercury salts
Dissolve some small crystals of mercury nitrate in a small amount of water. Note the formation of
a precipitate (or turbidity) due to the formation of a basic salt. Test the digestion reaction using red
and blue litmus paper. Write the equation for the hydrolysis reaction.
13. Preparation of calomel
To the solution of mercuric nitrate add the solution of sodium chloride or hydrochloric acid. A
white precipitate of Hg2Cl2 is formed. Write the reaction equation.
14. The action of potassium iodide on mercury salts.
Add a little of the potassium iodide solution to the mercuric nitrate solution. A yellow to green
precipitate of Hg2I2 is formed. Write the reaction equation.
By adding excess potassium iodide, the precipitate dissolves forming K2[Hgl4] and metallic
mercury which appears as a brown or black precipitate. Write the reaction equation.
15. Oxidation of mercury salts
Mix a small amount of mercuric nitrate solution in a porcelain beaker with a few drops of
concentrated nitric acid. Prove that after this there are mercuric ions (Hg2+) in the solution. Write
the equation for the oxidation reaction of mercuric nitrate.
Lab 15-IRON. CHROME. MANGANESE.
Chromium
101
Chromium belongs to group VI B of the periodic system. Unlike the elements of the oxygen group
(VI A) this is a metal, which is determined by the structure of its atom. Chromium in the outer
shell contains one electron, therefore it does not withdraw electrons, but it can donate a maximum
of 6 electrons (1 from the outer shell and 5 from the penultimate shell not filled with 13 electrons).
So, in its composition, chromium has only the positive valence that varies from 2 to 6. Of particular
importance are the trivalent and hexavalent chromium compounds. The latter closely resemble the
corresponding sulfur compounds.
Chromic oxide CrO is a basic oxide, chromic oxide Cr2O3 has amphoteric, basic and acidic
properties, while chromic anhydride CrO3 is an acidic oxide.
Chromic oxide is a green substance that melts with difficulty and is insoluble in water and acids.
The hydrate corresponding to this Cr(OH)3 oxide has an amphoteric character. It dissolves in
acids, forming trivalent chromium salts, and in alkalis, forming orthochromic (H3CrO3) or
metachromic (HCrO2) acid salts, which are called chromites.
Most Cr salts are soluble in water. Their solutions depending on the conditions have different
colors. When cooled these usually turn blue to purple, while when heated they turn green. Such a
color change depends on the different hydration of the Cr3+ ion (see work No. 16). Trivalent
chromium has a great tendency to form complex compounds with coordination number 6, for
example [Cr(NH3)6]Cl3.
Soluble salts of Cr3+ and chromite in aqueous solutions are hydrolyzed. Chromic anhydride is a
red substance with very strong oxidizing properties, it is produced during the action of
concentrated sulfuric acid on chromic acid salts. Chromic anhydrite corresponds to chromic acid
H2CrO4 and dichromic acid HI2Cr2O7. These acids are known only in digestion and are quite
strong. Chromic acid salts (chromates) have a yellow color, which is the characteristic color of the
CrO42 ion, while dichromic acid salts (dichromates) have an orange color, which is the
characteristic color of the Cr2O,2 ion. Most chromates and dichromates are insoluble in water.
In solutions of chromate and dichromate salts, this balance is established:
Cr2O22+H2O=2CrO42+2H+ +H2O→2CrO42+2H+
By adding acid, this balance shifts to the side of dichromate formation (to the left), while by
adding alkali, it shifts to the side of chromate formation (to the right).
Trivalent chromium salts under the influence of oxidizing substances are oxidized to hexavalent
chromium compounds. The alkaline environment helps this process, which can also be seen in this
example:
NaCrO2+3Br2+8NaOH=2Na2 CrO4+6NaBr+4H2O or in ionic form:
2CrO2+3Br2+8OH=2CrO42+6Br +4 H2O
102
Hexavalent chromium compounds in an acid environment are strong oxidizing substances, for
example:
or in ionic form;
Cr2O22+6Br+14H+=2Cr3++3Br2+7H2O
By the action of very strong reducing agents such as (NH4)2S, hexavalent chromium compounds
turn into trivalent chromium compounds even in a neutral or weakly alkaline environment.
Apparatus: 1) tripod with clips; 2) lamps; 3) porcelain cups; 4) unbaked clay dishes; 6) 100 ml
beaker; 7) funnel; 8) test tube holders; 9) small porcelain spoon; 10) iron fence; 11) iron wire or
large nails.
Reagents and materials: 1) ammonium dichromate (NH4)2 Cr2O7; 2) ethyl alcohol C2HsOH. 3)
filter paper; 4) glass wool or friable abscess; 5) chromium sulfate Cr2(SO4)3; 6) potassium
carbonate K2CO3 or potassium hydroxide KOH; 7) potassium nitrate or chlorate KNO3 or KCIO3
8) chromium oxide Cr2O3.
Solutions: 1) sulfuric acid H2SO4 (concentrated and 2 normal); 2) hydrochloric acid HCl
(concentrated and 2 normal); 3) sodium hydroxide NaOH (2 normal); 4) ammonium sulfide
(NH4),S; 5) barium chloride BaCl2 (1 normal); 6) potassium chromate K2CrO4 (l normal); 7) two
potassium chromates K2Cr2O7 (saturated and 0.5 normal); 8) sodium nitrate NaNO2 (1 normal);
9) sodium sulfite Na2SO3 (1 normal); 10) silver nitrate AgNO3 (0.1 normal), 11) bromine water;
12) hydrogen peroxide H2O2 (3%).
Practical work
1. a) Pour some crushed ammonium dichromate into a test tube and fix it obliquely on the tripod.
Do not point the nozzle of the test tube at yourself or at other people nearby. Heat the top layer of
salt until the reaction starts and then suspend the heating. Explain the phenomenon that occurs.
b) Treat the obtained green powder of chromium oxide with water and sulfuric acid or dilute nitric
acid. Does chromium oxide dissolve in water and dilute acids?
2) Preparation and properties of chromium hydroxide
a) To a test tube containing a solution of one of the chromium alums, add the sodium hydroxide
solution dropwise until an ash-green precipitate of chromium hydroxide forms. Write the reaction
equation.
b) Divide the obtained precipitate into two test tubes. Add dilute acid to one of them, and an excess
of alkali to the other until the precipitate is completely dissolved. Write the equations of the
reactions.
c) Bring the resulting chromite solution to boil. Explain the formation of chromium hydroxide
precipitate. Write the reaction equation.
103
3. Hydrolysis of chromium salts
To the solution of one of the chromium salts, add the solution of ammonium sulphide. Observe the
formation of an ash-colored precipitate in the jeskil. Filter the obtained precipitate and rinse well
with water on the filter.
Half of the precipitate is added to a test with dilute hydrochloric acid, while the other half is a
solution of some alkali. In both test tubes, the precipitate dissolves, and in the first one, hydrogen
sulphide gas is not released. Based on the reactions done, draw the conclusion that the precipitate
obtained is or is not the salt of hydrogen sulphide. Write the equations of the reactions.
4. Oxidation of trivalent chromium salts.
a) Take 2-3 ml of a solution of one of the chromium bases and dilute with excess alkali until
chromite is formed, then add bromine water. Heat the mixture. Note the change in the color of the
solution from the green color characteristic of the CrO2- ion to the yellow color characteristic of
the CrO42 ion. Write the reaction equation in molecular and ionic form.
b) Melt 1-2 g of potassium carbonate (or potassium hydroxide) with 0.5-1 g of potassium nitrate
or chloride in an iron pot. In the melt, throw, carefully, a few crystals of chromium sulfate (or a
little chromium oxide powder) and mix the mass well with an iron wire (or nail). Heat the pan
again on a strong flame for 10-15 minutes. After cooling, dissolve the obtained melt in water. Note
the yellow color of the potassium chromate. Write the reaction equation.
5. Preparation and properties of chromic anhydrite
a) Pour 3-5ml of saturated potassium dichromate solution into a beaker (or test tube) and add little
by little 5-8ml of concentrated hydrogen sulphide, cooling the beaker with cold water. Dark red
crystals of chromic anhydrite are formed. After cooling the solution, filter the obtained crystals
through asbestos or glass filter layers. Write the reaction equation.
b) Place the obtained crystals in a porcelain bowl and moisten them with a pipette with a few drops
of alcohol. The latter catches fire and partially burns. During the oxidation of alcohol, compounds
of trivalent chromium with a green color and acid with a characteristic smell of vinegar are formed.
6. Transition from chromate to dichromate and vice versa.
a) To the solution of K2CrO4, add the solution of any acid.
Note the color change. Explain the phenomenon that develops. Write the reaction equation.
b) To the solution of K2Cr2O7, add the solution of some alkali.
Note the color change of the solution. Explain this difference. Write the reaction equation. What
ions are found in aqueous solutions of chromate and dichromate?
7. Reactions for CrO2 and Cr2O
104
a) Put the solution of K2CrO4 in a test tube and the solution of K2Cr2O7 in another test tube. Then
add the AgNO3 solution to both test tubes. Note that in both cases the same crimson precipitate of
Ag2CrO4 will form. In the case of K2Cr2O, this is explained by the fact that Cr2O22 and CrO42
ions are found simultaneously in its solution and that the solubility product of Ag2CrO4 is smaller
than that of Ag2Cr2O7 (see table 9).
b) Do the same experiment taking instead of the solution of AgNO3, the solution of BaCl2. Note
the formation of the yellow precipitate of BaCrO4 in both cases. Write the equations of the
reactions.
8. Oxidizing properties of hexavalent chromium salts.
a) Add dilute sulfuric acid and NaNO2 solution to 2-3 ml of K2Cr2O7 solution. Heat this mixture
gently. Note the color change from orange (Cr2O7) to green (Cr3+). Write the reaction equation
in molecular and ionic form.
b) Add 2-3 ml of the potassium dichromate solution to the ammonium sulphide solution. Note the
formation of chromium hydroxide precipitate. Write the reaction equation.
9. Preparation and decomposition of perchromic acid.
Pour into a test tube 2-3 ml of diluted sulfuric acid and the same amount of 3% hydrogen peroxide
solution. Pour a few drops of potassium chromate or dichromate solution into this test tube, mixing
well. Note the color change from yellow or orange to blue due to the formation of perchromic acid.
Over time notice the change in color of the solution from blue to green again, due to the
decomposition of the perchromic acid. Write the equations of the reactions.
Manganese
Manganese is an element of the group VII B of the periodic system. In the outer shell, its atom has
two electrons and in the penultimate one there are 13. It can release not only the two electrons of
the outer shell, but also five electrons from the outer shell. penultimate unfilled. This element does
not have the ability to attract electrons, therefore manganese is distinguished from the halogens
that are in group VII A. So manganese in its compounds only has the positive valence 2,4,6 and 7.
As the valence of manganese increases, the basic properties of its oxides weaken and the acidic
ones strengthen. Both the lowest manganese oxides—manganous oxide MnO and manganese
oxide Mn2O3—as well as their corresponding hydrates Mn(OH)2 and Mn(OH)3 have basic
properties. Manganese dioxide MnO2 and its hydrates Mn(OH)4 and H2MnO3 are amphoteric
substances. Magnetic anhydride MnO3 and permanganic Mn2O7 as well as their hydrates
H2MnO4 (manganic acid) and HMnO4 (permanganic acid) have acid character.
The white, water-insoluble hydrate of manganese oxide is readily oxidized in air to the dark brown
hydrate Mn(OH)4. Divalent manganese salts, as well as their aqueous solutions, are mostly pale
rose in color. These are the most stable manganese compounds in the acidic environment. By the
105
action of strong oxidizers, divalent manganese compounds can be oxidized to compounds with
higher valence.
Manganese dioxide is a black substance that does not dissolve in water, it is the most stable
compound of manganese with oxygen under ordinary conditions. In an acidic environment, MnO2
is an oxidizing substance and is reduced by itself to divalent manganese salts. By the action of
stronger oxidizing substances MnO2 can be oxidized to hexavalent and heptavalent manganese
compounds.
During the fusion of MnOz or divalent manganese salts with alkalis and an oxidizing substance
such as KCIO3, KNO3, etc., manganese acid salts (manganates) are formed. These have a dark
green color, characteristic of the MnO42 ion.
Manganates are more or less stable only in highly alkaline environments. In dilute solutions, these
decompose into MnO2 and permanganic acid salts (permanganate) according to this equation:
By acidifying solutions of manganates, H2MnO4 is produced, which is very unstable and

immediately decomposes according to the equation:
All hexavalent manganese compounds are strong oxidizers and are easily reduced to MnO2 in
neutral and alkaline environments or to Mn2+ salts in acidic environments. Under the action of
strong oxidizing substances (for example Cl2,HNO3) they can turn into heptavalent manganese
compounds. Permanganic acid HMnO4.
Recognized only in digestion. Solutions of permanganic acid and its salts (permanganates) have a
violet-red color that is characteristic of the MnO4 ion. During heating, the permanganates
decompose easily, releasing oxygen. Permanganic acid and its salts are powerful oxidizing
substances. In an acidic environment, these are reduced to divalent manganese salts, while in a
neutral (neutral) and weakly alkaline environment, they are reduced to MnO2. If the environment
is strongly alkaline and the reducing agent is taken in small quantities, then the permanganates are
reduced at first to manganates which then slowly change to MnO2.
Apparatus and containers: 1) stand with clamp; 2) light bulb; 3) test tube holder, 4) watch glass;
5) glass birch; 6) small graduated cylinders with pupils (10, 50, 100 ml).
Reagents and materials: 1) lead dioxide PbO2 (or minimum Pb3O4); 2) manganese dioxide
MnO2 (granulated); 3) potassium hydroxide KOH; 4) Bertole's salt KC103; 5) manganese sulfate
MnSO4. 7H2O; 6) potassium permanganate KMnO4; 7) litmus paper; 8) birch wood; 9) alcohol
C2HsOH; 11) cotton.
Solutions: 1) nitric acid HNO3 (concentrated); 2) sulfuric acid H2SO4 (concentrated and 2
normal); 3) sulfuric acid H2SO3; 4) acetic acid CH3COOH (2 normal); 5) sodium hydroxide
NaOH (40% and 2 normal; 6) ammonium sulphide (NH4)2S; 7) potassium permanganate KMnO4
(0.1 normal); 8) manganese sulfate MnSO4 (0.5 normal); 9) sodium sulfite Na2SO3(1 normal);
10) chlorine water; 11) bromine water (2 normal).
Practical work
106
1. Preparation and properties of manganese hydroxide
Add the sodium hydroxide solution to the manganese sulfate solution. A white precipitate of
divalent manganese hydroxide is formed. Write the reaction equation.
Pour a part of the liquid, together with the precipitate, into another test tube and let it stand in the
air. The precipitate slowly darkens. To speed up this process, shake the contents of the test tube
from time to time. Explain the change in the color of the precipitate. Write the reaction equation.
Divide a portion of the manganese hydroxide precipitate into two test tubes and add dilute acid to
one of them, while adding excess alkali to the other. Does this precipitate dissolve in both cases?
What can be concluded about the properties of manganese hydroxide? Write the reaction equation.
2. Preparation of manganese sulphide
Add the ammonium sulfate solution to the manganese sulfate solution. Note the formation of flesh-
colored precipitate of manganese sulfide. In the air it darkens slowly because it oxidizes to
Mn(OH)4. Write the reaction equation.
Test the behaviour of the obtained precipitate of MnS against dilute acids. Write the reaction
equations.
3. Oxidation of manganese salts
a) Add sodium hydroxide solution and bromine water to the manganese sulfate solution. Heat the
sample. Explain why the precipitate turns brown. Write the equation in molecular form and in
ionic form.
b) Put some minium Pb3O4 or lead dioxide PbO2 in a test tube, add 2-3 ml of concentrated nitric
acid and 2-3 drops of manganese sulfate solution. Heat the mixture to a boil. After depositing the
undissolved particles note the purple to red color of the HMnO4 solution. Write the reaction
equation.
c) Pour 2-3 drops of manganese sulfate solution, 1-2 ml of silver nitrate solution (as a catalyst), 1-
2 concentrated sulfuric acid and 3-4 ml of ammonium persulfate solution into a test tube. Carefully
heat the sample until the solution turns red-purple due to the formation of permanganic acid. Write
4. Interaction of manganese dioxide with sulfuric acid
Add a little concentrated sulfuric acid to a small amount of granular MnO2. Heat the test tube
containing the mixture carefully until a violent gas is released. Prove that this gas is oxygen. Write
the reaction equation. What properties does MnO2 have in this reaction?
5. Preparation of potassium manganate
In a test tube, melt little by little Bertollet's salt together with a piece of potassium hydroxide and
a few crumbs of manganese dioxide or manganese sulfate. Melt. green obtained after cooling,
107
dissolve in a small amount of water. A green potassium manganate solution is formed. Write the
reaction equation. What properties do MnO2 and MnSO4 have in this reaction? Save the solution
for future experiments.
6. Decomposition of manganic acid.
Add dilute acetic acid to a small amount of the potassium manganate solution obtained in
experiment 5. Note the change in color of the solution from green to purple to red and the formation
of a brown precipitate of MnO2 Explain the observed phenomenon. Write the equations of the
reactions.
7. Oxidation of potassium manganate
To a portion of the green solution of K2MnO4, obtained in experiment 5, add chlorine water little
by little until it changes color from purple to red. Explain the observed phenomenon. Write the
reaction equations.
8. Oxidizing properties of potassium manganate
a) To the solution of potassium manganate, obtained in experiment 5, add the solution of Na2SO3
and heat it. Note the formation of a brown precipitate of MnO2. Write the reaction equation.
b) Add sulfuric acid solution to a small amount of potassium manganite solution until an acid
reaction is created (litmus paper test). Note how the color of the digest disappears. Write the
reaction equation.
How does the reaction of the environment affect the reduction process of K2MnO4?
9. Decomposition of potassium permanganate
Heat a small amount of KMnO4 crystals in a test tube. Test their oxygen release. Continue heating
until the evolution of oxygen ceases. After cooling, dissolve the contents of the test tube in a small
amount of water. Note the formation of a green solution of K2MnO4 and a brown precipitate of
MnO2. Write the reaction equation.
10. Oxidizing properties of potassium permanganate
a) Pour 1-2 ml of KMnO4 solution into three test tubes. Then add dilute sulfuric acid to one, water
to the other and a concentrated solution of some alkali to the third.
After that, add Na2SO3 solution to all test tubes. In the first test tube, the solution loses its color
(whitens), in the second, a brown precipitate of MnO2 is formed, and in the third, a green solution
of K2MnO4 is initially formed, which later turns into a brown precipitate of MnO2. Explain the
phenomena that occur and note the influence of the ambient reaction on the reduction of KMnO4.
Write the reaction equations in molecular and ionic form.
108
b) In a test tube, mix 3 ml of potassium permanganate with the same volume (3 ml) of manganese
sulfate solution (MnSO4). What will you notice? What reaction (pH) will the final solution have?
Test this with the litmus paper side. Write the reaction equation.
11. Interaction of permanganate with concentrated sulfuric acid.
Place 5-6 permanganate crystals in a watch glass and add a few drops of concentrated sulfuric acid
to them with a pipette. Since the resulting permanganic anhydride is a strong explosive, it is not
allowed to take larger quantities of permanganate and sulfuric acid. Mix these two (KMnO4 and
H2SO4) very carefully with a glass rod. Dampen a cotton ball with alcohol and bring it into contact
with the wet tip of the glass birch mixture. Note the ignition of the alcohol and write the reaction
equations.
Iron
Iron, cobalt and nickel form two types of oxides: FeO, CoO and NiO and the second type Fe2O3,
Co2O3 and Ni2O3.
The divalent hydroxides of these metals are insoluble in water, but dissolve well in acids because
they have weak basic properties. In air, Fe(OH)2 from white is easily oxidized to Fe(OH)3 with a
brown color. Oxidation of Co(OH)2 (rose-red) by air oxygen to Co(OH)3 (brown-brown) is
usually slow.
Almost all salts formed by these metals with strong acids are soluble in water. Hydrated ions of
Fe2+ are green, those of CO2+ are rose-red, while those of Ni2+ are light green. In aqueous
solutions, the soluble salts of these metals are hydrolyzed.
Ferric oxide and salts in the solid state and especially in solution are readily oxidized in air to ferric
(trivalent iron) salts. The greater the concentration of hydrogen ions in the solution, the slower
their oxidation. In a very acidic environment, ferrous compounds (of divalent iron) can be oxidized
only by the action of powerful oxidants.
Ferric hydroxide Fe(OH)3 has weak basic properties and even weaker acidic properties. It is
insoluble in water, but easily forms colloidal solutions in it. It dissolves well in acids. When heated,
it also dissolves in concentrated solutions of strong alkalis and forms ferric acid salts HFeO2 called
ferrites. Cobalt and nickel hydroxides are insoluble in water. During their dissolution in acids,
cobalt and nickel salts are not formed, but cobalt and nickel salts are formed and simultaneously
oxygen is released. The latter is released when substances that are capable of oxidation are missing.
Most ferric salts dissolve well in water. In aqueous digestion these are highly hydrolyzed. As a
result of hydrolysis, colloidal solutions of basic salts are formed that have a yellow to brown color,
while the Fe3+ ion itself has a green to yellow color.
Under the action of powerful reducing agents, ferric salts (of trivalent iron) are reduced to ferric
salts (of divalent iron). The greater the concentration of hydrogen ions in the solution, the easier
the reduction of ferric salts.
109
Iron, cobalt and nickel, as elements that have the penultimate layer incomplete; yield complex
molecules and ions. For cobalt compounds, the most stable complexes are only those where it is
trivalent. Therefore, complex compounds of divalent cobalt can also be oxidized
from air oxygen to trivalent compounds. The coordination number of Fe, Co and Ni is usually 6.
Apparatus and dishes: 1) apparatus according to fig. 53; 2) magnesium; 3) tripod with ring and
clip; 4) lamps; 5) porcelain pot with lid; 6) funnel; 7) 200 ml student glasses; 8) stand with test
tubes; 9) long test tubes; 10) porcelain triangles; 11) thick glass birch.
Reagents and materials: 1) iron (powder); wire or nail; 2) tin (pieces); 3) zinc (pieces) 4) ferric
oxide Fe2O3; 5) ferric chloride FeCl3 6) calcium chloride CaCl2; 7) cobalt nitrate Co(NO3)2
6H2O; 8) ethyl alcohol C2H3OH; 9) steel pen tip 2 pieces; 10) filter paper; 11) litmus paper; 12)
zumper paper; 13) KOH potassium hydroxide.
Solutions: 1) nitric acid HNO3 (concentrated fuming and 2 normal); 2) sulfuric acid H2SO4
(concentrated 2 normal); 4) hydrochloric acid HC1 (concentrated and 2 normal) 4) acetic acid
CH3COOH (2 normal);5) sodium hydroxide NaOH (40% and 2 normal) 6) ammonium hydroxide
NH4OH (2 normal); 7) ammonium sulfide (NH4)2S; 8) ammonium chloride NH4Cl (2 normal);
9) Ferrous sulfate FeSO4 (0.5 normal) (freshly prepared); 10) ferric chloride FeCl3 (0.5 normal);
11) potassium nitrate KNO3; 12) potassium ferrocyanide. K4[Fe(CN)6];13) potassium
ferricyanide K3[Fe(CN)6];14) potassium iodide KI (0.1 normal); 15) potassium permanganate
KMnO4 (0.1 normal); 16) potassium sulfocyanide KSCN (0.5 normal); 17) potassium dichromate
K2Cr2O7 (0.5 normal); 18) cobalt chloride CoCl2 (concentrated with 0.5 normal; 19) copper
sulfate CuSO4 (0.5 normal); 20) sodium carbonate Na2CO3 (2 normal); 21) nickel sulfate NiSO4
(0.5 normal); 22) bromine water; 23) sulphidic water; 24) stannous chloride SnCl2 (0.5 normal);
25) barium chloride BaCl2 (2 normal); 26) dimethyl-glyoxin (alcoholic solution).
Practical work
1. Reduction of iron oxide
Pour some ferric oxide into a test tube and then fix the test tube horizontally on a tripod. Open the
tube of the apparatus to the readiness of the hydrogen, and after it is connected with the hydrogen
which is pure, the appearance of the outgassing in the test-tube which has no oxidation of iron.
After a minute, start heating the test and notice the color change of Fe2O3. When all the powder
has been blackened the heating, while the hydrogen extraction continues until the test tube is done.
After cooling the test tube, pour the obtained iron on a sheet of paper and test its position as well
as that of Fe2O3 against the magnet. Write the reaction equation.
2. Grinding of iron
Place a thin piece of zinc in the crack of the steel pen tip, and a piece of tin in another pen tip. Pour
water into two test tubes and add 2-3 drops of dilute sulfuric acid and the same amount of
potassium hexacyanoferrate III or potassium ferricyanide K3[Fe(CN)6] which is an extremely
sensitive reagent. The hexationoferrate ion with the Fe2+ ion forms a blue complex compound.
Put the two pens together with the two pieces of metal into two test tubes that have a prepared
solution. The liquid in which the pen with the piece of tin is immersed turns blue after a few
110
minutes, which indicates corrosion of the iron. In the other test tube, the blue color can be observed
only after all the zinc has been dissolved. Consider all the reactions that take place, taking into
account the place that Fe, Zn and Sn occupy in the range of metals. Give the scheme of grating of
galvanized iron and wrought iron
3. Interaction of iron with acids
(Do the work in the gas cupboard)
Dilute and concentrated acids such as HCI, H2SO4 and HNO3 were added to small amounts of
iron powder placed in separate test tubes. Heat the sample where the reaction does not take place
in the cold. Notice the phenomenon that occurs. Write the equations of the reactions.
4. The passivity of iron
Pour fuming nitric acid into a wide test tube and dip a well-cleaned iron wire (or a nail) into it.
After 1-2 minutes, remove the wire carefully without touching the sides of the test tube. Rinse the
wire or nail with water to remove the acid and place it in the copper sulfate solution for a few
seconds. Take the iron out of the solution, and you will see how no copper has settled on it. Then
hit the wire (or nail) hard with a thick glass rod and dip it again in the copper sulfate solution. Note
the separation of copper. Explain why, after treatment with concentrated nitric acid, copper does
not separate from iron. What is the meaning of hitting the wire (iron) on the side of the birch?
5. Preparation and properties of ferric hydroxide
To the freshly prepared solution of ferrous sulfate (obtained by dissolving iron powder obtained
in excess in dilute sulfuric acid H2SO4) add the solution of sodium hydroxide. Note the formation
of almost white precipitate of ferric hydroxide. Write the reaction equation.
Staying in the air, the precipitate changes its color, due to oxidation, and slowly turns from dark
green to black and finally from brown to red. Write the equation for the oxidation reaction of
ferrous hydroxide to ferric hydroxide.
Test the behavior of Fe(OH)2 against dilute hydrochloric acid and against excess alkali. Write the
reaction equation. What properties does ferric hydroxide have?
6. Preparation of ferrous sulphide
To the solution of ferrous sulfide, add the solution of ammonium sulfide. Note the formation of a
black precipitate of ferrous sulfide. Write the reaction equation. Test the behaviour of the
precipitate against dilute acids. How does hydrogen sulfide gas dissolve ferrous sulfate? Explain
the difference in the action of sulphide and hydrogen sulphide gas on the dissolution of ferrous
sulphate.
7. The reaction for the detection of the Fe2+ ion
111
To the solution of ferrous sulfate add the solution of potassium hexazioneferrate III or potassium
ferricyanide K3[Fe(CN)6]. A blue precipitate of Fe3[Fe(CN)6]2 is formed. Write the reaction
equation.
8. Preparation and properties of ferric hydroxide
a) Add the sodium hydroxide solution to the ferric chloride solution. A reddish brown gelatinous
precipitate of Fe(OH)3 is formed. Test the reaction of this precipitate to acids. Write the equations
of the reactions.
Freshly precipitated ferric hydroxide Fe(OH)3 is partially dissolved in concentrated, warm alkali
solutions. What properties does hydroxide have?
b) Prepare the Fe(OH)3 precipitate again. Filter and rinse with water over the filter. Then place the
filter paper on a porcelain bowl and wring it out. Brown to red ferric oxide is formed. Write the
reaction equation.
9. Hydrolysis of ferric salts.
a) Dissolve a small amount of ferric chloride in water. Determine the dissolution reaction using
litmus. Write the equation for the hydrolysis reaction. Add soda solution to the solution of ferric
chloride. Note the formation of ferric hydroxide precipitate and the evolution of carbon dioxide.
Write the reaction equation. How can it be pointed out that the precipitate obtained is not a salt of
carbonic acid?
10. Formation of ferric sulfide.
Add ammonium sulphide solution to the ferric chloride solution. A black precipitate of Fe2S3 is
formed. Write the reaction equation.
11. The reaction for the detection of the Fe3+ ion
a) To the solution of ferric chloride add a solution of hexacyanoferrate II transition or potassium

ferrocyanide K4[Fe(CN)6]. A blue precipitate of Prussian blue Fe4[Fe(CN)]3 is formed. Write the
reaction equation.
12.Oxidation of divalent iron.
a) Add dilute sulfuric acid, a little concentrated nitric acid to the solution of ferrous sulfate and
heat until it boils. Write the reaction equation.
b) Add dilute sulfuric acid and bromine water to the ferrous sulfate solution. Write the reaction
equation.
c) Add dilute sulfuric acid and a few drops of KMnO4 or K2Cr2O7 solution to the ferrous sulfate
solution. Write the reaction equation. Note that in all three test tubes the Fe2+ ion is oxidized to
the Fe3+ ion.
112
13. Reduction of trivalent iron.
a) Add hydrogen sulfide water to the solution of ferric chloride. Turbidity of the liquid occurs, due
to the separation of sulfur. Write the reaction equation. Note the presence in the solution of ferric
(divalent iron) ions.
b) Add potassium iodide solution to the solution of ferric chloride. Explain the color change. Write
c) To the acidified solution of ferric chloride, add stannous chloride solution (of divalent tin) drop
by drop. Note the color change and write the reaction equation.
14. Preparation of ferratas
In a porcelain pot take a small amount of crushed potassium hydroxide, some ferric oxide powder
(or some ferric salt) and some potassium chlorate. Mix the three substances carefully. Place the
pot on a tripod, on a porcelain triangle.
113
ANNEX
SOLUBILITY OF SALTS AND BASES IN WATER
Cation/Anion Na+ K Ag Mg2+ Ca2+ Sr2 Ba+ Zn x Pb2+
F 4,44 92,56 195,4 0,0076 0,0016 0,0012 0,16 0,005 0,07
CI 35,86 32,95 0,0316 55,81 73,19 51,09 37,24 203,9 1,49

Br 88,76 65,86 0,041 103,1 143,3 96,52 103,6 478,2 0,598
I 177,9 137,5 0,0635 148,2 200 169,2 201,4 419,0 0,08
NO5 83,97 30,34 213,4 74,3 121,8 66,27 8,74 117,8 51,66
C105 97,16 6,6 12,25 126,4 179,3 174,9 35,42 183,9 150,6
SO2 16,83 11,11 0,55 35,43 0,20 0,011 0,0323 53,12 0,0041
CO3- 16,39 108,0 0,003 0,1 0,0013 0,0011 0,0023 0004 0,031
Cro2- 61,21 63,1 0,0025 73,0 0,4 0,12 0,0338 - 0,042
Cr2O,2- 3,34 30,27 0,0035 0,03 0,0356 0,0046 0,0086 0,036 0,0315
.HO 116,4 142,9 0,01 0,001 0,17 0,77 3,7 0,035 0,01
114
115

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LAB MANUAL-GENERAL & INORGANIC CHEMISTRY- EXPERIMENTS AND ACTIVITIES

2. Lab 2-Acids, bases and salts

3. Lab 3- Law of conservation of mass

4. Lab 4-Solutions, concentrations of solutions and preparation of solutions in the laboratory.

5. Lab 5-Electrolytic decomposition

6. Lab 6-Chemical equilibrium in electrolyte solutions

7. Lab 7-Hydrolysis of salts and colligative properties

8. Lab 8-Hydrogen, hydrogen peroxide. Oxygen.

9. Lab 9-Halogens.( chlorine and hydrochloride gas)

10. Lab 10-Boron, aluminium, carbon and silicon.

11. Lab 11-Alcaline metals. Magnesium and alkaline earth metals.

12. Lab 12-Oxygenated compounds of nitrogen. Phosphorus.

14. Lab 14-Copper and silver. Zinc, Cadmium, Mercury

15. Lab 15-Iron. Chrome. Manganese.

Literature for students on the development of laboratory classes:

MSc. Ergi HOXHA wbu. 2023

Lab Report Template

THIS LAB REPORT MUST BE TYPED IN ORDER TO RECEIVE CREDIT

MSc. Ergi HOXHA wbu. 2023

Lab 1-RULES OF TECHNICAL INSURANCE. SEPARATION OF THE COMPONENTS

Lab Safety Rules and Guidelines

2. Ensure you are fully aware of your facility's/building's evacuation procedures.

MSc. Ergi HOXHA wbu. 2023

10. Always work in properly-ventilated areas.

12. Laboratory glassware should never be utilized as food or beverage containers.

17. Do not work alone in the lab.

18. Never leave an ongoing experiment unattended.

20. Never smell or taste chemicals.

21. Do not pipette by mouth.

MSc. Ergi HOXHA wbu. 2023

Housekeeping safety rules

1. Always keep your work area(s) tidy and clean.

5. Solids should always be kept out of the laboratory sink.

MSc. Ergi HOXHA wbu. 2023

Dress code safety rules

1. Always tie back hair that is chin-length or longer.

4. Never wear shorts or skirts in the lab.

MSc. Ergi HOXHA wbu. 2023

Personal protection safety rules

4. Before leaving the lab or eating, always wash your hands.

MSc. Ergi HOXHA wbu. 2023

Chemical safety rules

1. Every chemical should be treated as though it were dangerous.

6. Do not put unused chemicals back into their original container.

7. Chemicals or other materials should never be taken out of the laboratory.

8. Chemicals should never be mixed in sink drains.

9. Flammable and volatile chemicals should only be used in a fume hood.

10. If a chemical spill occurs, clean it up right away.

11. Ensure that all chemical waste is disposed of properly.

MSc. Ergi HOXHA wbu. 2023

Chemistry lab safety rules

3. Always pour chemicals from large containers to smaller ones.

5. Never tap flasks that are under vacuum.

6. Chemicals should never be mixed, measured, or heated in front of your face.

Electrical safety rules

MSc. Ergi HOXHA wbu. 2023

2. High-voltage equipment should never be changed or modified in any way.

6. Whenever you can avoid using extension cords.

Laser safety rules

4. Always keep the laser beam at or below chest level.

MSc. Ergi HOXHA wbu. 2023

6. Do not walk through laser beams.

To separate the components of a mixture using the following techniques:

Lab Manual-General & Inorganic Chemistry WBU

Lab Manual-General & Inorganic Chemistry WBU