Cover page

Table of contents
Hazard Symbols
General Safety Rules

1. Make sure you are familiar with all the safety information given to you about each
experiment before starting the experiment. This includes your manual, these safety
guidelines, any posted information or any other information provided to by your TA.

2. Always wear safety glasses (including during check-in and check-out), except when their
removal has been specifically authorized by the TA prior to their removal. Contact lenses
are forbidden. You must also wear a face shield when requested to by the TA.

3. You must wear a lab coat (and do it up) in all Chemistry labs.

4. Footwear must completely cover the foot and heel (no sandals, baby dolls, ballet flats,
mules, open-toed footwear, etc.).

5. You must wear long pants (no shorts, capris, skirts, or dresses).

6. If you arrive at your Chemistry lab and do not have the required clothing, you will be
directed to rent or purchase missing items (glasses, lab coats, disposable foot coverings and
long pants) from Chemistry Stores before you will be allowed to participate in the lab.

7. Loose hair must be tied back so as to be out of the way. Dangling jewellery must be
removed.

8. Do not eat or drink in the lab.

9. Visitors are not allowed to be in the lab.

10. Please keep your work area and the common work areas tidy. Also, please make sure the
aisles, safety showers, eyewash stations and doorways are unobstructed.

11. Please leave all glassware, equipment, tools, etc. as clean or cleaner than you found them.

12. Please clean up spills immediately. If the spill is large or is of a hazardous material, inform
the TA immediately. Use spill mix to absorb solvent or caustic liquids.
 13. Please dispose of waste properly and in a timely manner and according to the instructions
provided in your lab manual. If you are not sure, please ask your TA for the proper method
of disposal.

14. Wash your hands before you leave the lab.

15. Do not remove chemicals or equipment from the lab except when required to do so for
analysis.

16. Please notify your TA of any serious medical conditions.

17. Do not wear ear buds or earphones while in the lab.

Chemical Safety

1. The vapors of many organic solvents are flammable or combustible. Do not expose electric
sparks, open flames and heating elements to organic solvent vapors. Unless otherwise
stated, assume all organic solvents are flammable.

2. Many chemicals (solid, liquid or vapor) are poisonous. Do not taste chemicals. If it is
necessary to smell a chemical, do so by fanning the vapors towards your nose. Never inhale
directly. Avoid inhaling dust or fine powders. Use fume hoods and personal protective
equipment when necessary.

3. Do not pipette with your mouth.

4. Be extremely careful when transferring, distilling or refluxing volatile liquids.

5. Do not return used chemicals back to the stock container.

6. Do not tap flasks under vacuum.

7. Do not heat, measure or mix any chemicals in front of your face.

8. Never heat a closed system – it will act as a bomb!

9. Never pour water into concentrated acid. Pour acid slowly into water, stirring constantly.
Mixing acid with water is often exothermic.
10. Concentrated acids and bases are stored in the fume hood. Do not carry them to your
bench.

11. Make sure test tubes containing reactions are pointed away from people, especially when
they are being heated. Pressurized gas cylinders must only be operated by the TA.
General Laboratory Equipment’s (Glass wares)
 Modern Periodic Table
PERIODIC TABLE
Laboratory Report Format

1. Title: Create a title in less than ten words that reflects the factual content of your report.

2. Objective: This section states the purpose of your experiment. Be specific about the outcomes
that you plan to achieve when you designed your experiment.

3. Theory: this section gives general definition about all the contents.

4. Materials used: Describe the substances, equipment and instrumentation that is to be used in
your work. Copy the format for this section from your laboratory manual or from the standard
procedure supplied by the teacher.

5. Procedure: Describe how you performed the experiment, and mention each step in
chronological order.

6. Data/Observations: This section demonstrates that you carried out an experiment carefully and
knowledgeably. The person reading your report should find it clear and convincing enough to take
your experimental results seriously.

7. Result and Discussion: In this section of the report, present your results and discuss them. Also
report possible errors in the procedure and results, including possible inaccuracies.Include any
problems that you encountered during your work. Present them objectively. If possible suggest
ways in which such problems could be reduced at least if not overcome.

8. Conclusion: This section should be brief, as it refers back to the objectives and considers how
and to what degree they have been met. Review the purpose of the experiment, and summarize the
implications of the results.
EXPERIMENT 1: Preparation of Hydrogen Gas/ Single Displacement
Reaction

Objective: To investigate the displacement reaction between magnesium/zinc with strong acids
(hydrochloric acid) and detect the formation of hydrogen gas

Theory

A reaction in which one element displaces another element from its compound is known as single
displacement or replacement reaction. A more reactive element displaces a less reactive element
from a compound. Example active metals displace hydrogen from acids. Reactive metals such as
potassium, calcium, sodium, magnesium and zinc displace hydrogen gas from dilute acids. For
example, zinc is an active metal, and it displaces hydrogen from hydrochloric acid; but copper
metal cannot do so due to its reactivity.

How can pure hydrogen gas be prepared and detected? Hydrogen can be made by reaction of any
active metal like Mg or Zn with a strong acid such as sulphuric acid or hydrochloric acid.

Magnesium + hydrochloric acid gives hydrogen gas + magnesium chloride

Since hydrogen gas is almost insoluble in water, it can be collected by displacement of water using
an inverted bottle.

Chemical and apparatus

HCl solution, Mg metal /Zn metal, distilled water, thistle tube, erlimeneyer flask, water trough,
spatula, measuring cylinder, matches
 Procedures
The trough is filled with water, and a wide mouth bottle is completely filled with water and
inverted on the shelf. Magnesium or Zink metal is placed in the bottom of the flask and the
acid (3M HCl) is introduced through the thistle tube ( which is just a long stemmed funnel).
Fill the flask with enough solution to cover the bottom of the thistle tube as shown to
prevent air from entering and hydrogen escaping through the funnel. Hydrogen gas will
begin to escape from the rubber tube ; allow the reaction to run for a few minutes before
connecting it to the inverted bottle as shown, to sweep air out of the flask. The collected
hydrogen will be saturated with water vapor and contaminated with small amounts of air.
You can force the through a tube packed with calcium chloride pellets to remove the water.
Hydrogen can be further purified by exploiting the fact that the gas is extremely soluble in
many solid metals. The metal palladium is especially good at dissolving hydrogen. If the
gas is forced through a tube blocked by a membrane of palladium, hydrogen passes through
the membrane but the gaseous impurities do not. Observe the color of the gas .collect the
 gas, the way you did for collecting it in a jar or gas collector. Bring a lighted match stick
near the mouth of the gas collector.

Post lab. Questions

 Discus briefly about physical and chemical properties of hydrogen gas.

 Describe the applications of hydrogen gas.
 What does the formation of bubbles indicate?
 What sound do you hear when the burning splint is close to the mouth of the test
tube?

EXPERIMENT 2: Preparation of Carbon Dioxide Gas and Its Test

Objective: To demonstrate the laboratory preparation of carbon dioxide and to identify various
physical and chemical properties of carbon dioxide.

Theory

Carbon dioxide, CO2, is one of two oxides of the element carbon and is the main product oxide of
carbon formed from the combustion of hydrocarbon fuels. Carbon dioxide is present in the
atmosphere and is produced by respiration and combustion. However it has a short time in this
phase as it is consumed by plants during photosynthesis.
Some physical properties of carbon dioxide are:– Colorless, Odorless, Soluble in water, ethanol
and acetone, Melting point is -78°C, Boiling Point is -57°C and Some of chemical properties of
carbon dioxide are: Carbon dioxide is a covalent molecule, reacts with basic oxides to form salts,
reacts with bases it gives salt and water e.t.c.

Carbon dioxide is prepared by:-

 by treating any metallic carbonate with dilute mineral acids, or

 CaCO3 + 2 HCl ==> CaCl2 + H2O + CO2
 By heating carbonates of metals other than alkali metals.
 Heat
MgCO3 ==> MgO + CO2
Materials/ Apparatus:
Dilute hydrochloric acid (HCl), Lime water, magnesium ribbon, calcium carbonate (marble chips),
spatula, candle, thistle funnel, glass jar, U-tube, matches, flask.

Procedure:
 Add three spatulas full of calcium carbonate or calcium bicarbonate chips to the flask.
 Pour dilute hydrochloric acid into the top of the funnel; ensure that the liquid covers
the tip of the funnel in the flask.
 Perform these various tests on the gas collected and note your results;
1. Observe the color of the gas formed during the experiment.
2. Uncover one of the gas jars and use your hand to gently waft the gas towards the
nostrils .Note the smell.
3. Use a match to light a small piece of magnesium ribbon/candle/paper and place
in the gas jar. Note the results.
4. Collect and treat the gases with sodium hydroxide and note the results.
Post lab. Questions
 How carbon dioxide used as a source of fire extinguisher?
 Describe its advantages and disadvantages of carbon dioxide gas.
 What does the formation of bubbles in the conical flasks indicate?

EXPERIMENT 3: Precipitation Reaction

Objective: Identifying metal cations and non metal anions by using precipitation reactions
Theory
A precipitation reaction is a type of chemical reaction in which two soluble salts in aqueous
solution combine and one of the products is an insoluble salt called a precipitate. It is also the
creation of a solid from a solution. When the reaction occurs in a liquid solution, the solid formed
is called the 'precipitate'. The chemical that causes the solid to form is called the
'precipitant'. Precipitation reactions occur when cations and anions in aqueous solution combine
to form an insoluble ionic solid. Whether or not such a reaction occurs can be determined by using
the solubility rules for common ionic solids as below table:
Soluble compounds exceptions
All nitrates(NO3-),perchlorates(ClO4- No exceptions
),chlorates(ClO3-)and acetates(CH3COO_)
Most halides Those containing Ag+,Hg2+,Pb2+,(Pb2+ Is
Soluble In Hot Water).
Most sulphates Ba2+,Hg2+,Pb2+,Sr2+
Carbonates(CO32-),phosphates(PO43- All carbonates ,phosphates and sulphides of
),sulphides(S2-) of alkali metals and other elements are insoluble
ammonium ion(NH4+)
Sulphides of alkaline earth metals No exception
Transition metal hydroxides are insoluble in water.

If a solution of any soluble transition metal compound is mixed with sodium hydroxide
solution then we get a displacement reaction. The sodium is the more reactive metal, and
displaces the transition metal from its compound. The transition metal hydroxide is
produced as a result. As this is insoluble in water it appears as a solid in the liquid. A solid
produced in a liquid in this way is called a precipitate.

The colour of the precipitate indicates which transition metal ion was in the initial solution.

Examples

Transition metal ions in Precipitate formed when mixed with sodium Colour of the
solution hydroxide solution precipitate

Cu2+ Copper hydroxide Blue

Fe2+ Iron(II)hydroxide Grey/green

Fe3+ Iron(III)hydroxide Orange/red

Non-metal ions

Precipitate can be used to detect non- metal ions. Chlorides (Cl-),bromides(Br-) and iodides(I-)ions
make insoluble precipitates with silver ions(Ag+).each of these precipitates has a characteristics
colour as shown below

Ion tested Test Colour of the precipitate

- Acidify with dilute nitric acid ,add silver nitrate solution white
Cl (aq)

- Acidify with dilute nitric acid ,add silver nitrate solution cream
Br (aq)

- Acidify with dilute nitric acid ,add silver nitrate solution yellow
I (aq)

Chemicals and apparatus

Copper sulphate, iron (||) chloride, iron (|||) chloride, silver nitrate, sodium chloride, sodium
bromide, sodium iodide, sodium hydroxide solutions, distilled water, test tube, test tube holder,
test tube rack, measuring cylinder, potassium nitrate solution, barium nitrate solution, silver nitrate
solution, and nickel (II) nitrate solution, sodium sulfate solution, sodium phosphate solution.

Procedure 1

 Prepare 2M of copper sulphate, 1M of iron (||) chloride, and 1M of iron (|||) chloride
solutions. Pour those solutions to the separate test tubes and then add 0.1M sodium
hydroxide solution to each test tube. If desired, the mixture was heated gently to increase
rate of reaction or added in excess to detect further complex reactions, usually the
dissolving of the precipitate just formed. Record the color of the precipitate formed.
Write its chemical reactions.
  Prepare a solution which you want to test on presence of halide ions. For demonstration
take solutions of 0.25M potassium iodide, 0.25M sodium bromide and O.25M sodium
chloride.

 Pour solutions to the separate test tubes.

 Add a few drops of 0.1M silver nitrate solution in to those each test tubes containing
halides. If the solution under study contains halide ions the formation of a soft curdy
precipitate is observed. The precipitate color is specific to the type of ion (chloride,
bromide or iodide ion).

 Write down all the chemical reactions.

Procedure 2

1. Except for the laboratory handout, remove all books, purses, and such items from the laboratory
bench top, and placed them in the storage area by the front door. For laboratory experiments you
should be wearing closed-toe shoes. Tie back long hair, and do not wear long, dangling jewelry or
clothes with loose and baggy sleeves. Open you lab locker. Put on your safety goggles, your lab
coat, and gloves.

2. Place about 1 mL of potassium nitrate solution, barium nitrate solution, silver nitrate solution,
and nickel (II) nitrate solution into four separate small test tubes. Measure the 1 mL with a
graduated cylinder one time only, then approximate all further volumes. Add about 1 mL of sodium
acetate solution to each of the four test tubes. In boxes A to D of your Data Table, record S if the
resulting solution contains only soluble products, and I if the resulting solution contains an
insoluble product. Include the appearance of the insoluble product. If precipitates form, write and
balance the molecular, ionic, and net ionic equations in the Reaction Work section of your lab
report. Write the final net ionic equations under Reactions A to D in the Reactions section of your
lab report, or write NR for any mixture that did not form a precipitate. Save all solutions in a 400-
mL waste beaker on your lab bench and clean the four test tubes.

3. Refill the four test tubes as before with about 1 mL of potassium nitrate solution, barium nitrate
solution, silver nitrate solution, and nickel (II) nitrate solution. This time add about 1 mL of sodium
chloride solution to each of the four test tubes. In boxes E to H of your Data Table, record S if the
resulting solution contains only soluble products, and I if the resulting solution contains an
insoluble product. Include the appearance of the insoluble product. If precipitates form, write and
balance the molecular, ionic, and net ionic equations in the Reaction Work section of your lab
report. Write the final net ionic equations under Reactions E to H in the Reactions section of your
lab report, or write NR for any mixture that did not form a precipitate. Save all solutions in the
waste beaker on your lab bench and clean the four test tubes.

4. Refill the four test tubes with the metal ion solutions, and this time adds 1 mL of sodium sulfate
solution to each. In boxes I to L of your Data Table, record S if the resulting solution contains only
soluble products, and I if the resulting solution contains an insoluble product. Include the
appearance of the insoluble product. If precipitates form, write and balance the molecular, ionic,
and net ionic equations in the Reaction Work section of your lab report. Write the final net ionic
equations under Reactions I to L in the Reactions section of your lab report, or write NR for any
mixture that did not form a precipitate. Save all solutions in the waste beaker on your lab bench
and clean the four test tubes.

5. Refill the four test tubes with the metal ion solutions, and finally add 1 mL of sodium phosphate
solution to each. In boxes M to P of your Data Table, record S if the resulting solution contains
only soluble products, and I if the resulting solution contains an insoluble product. Include the
appearance of the insoluble product. If precipitates form, write and balance the molecular, ionic,
and net ionic equations in the Reaction Work section of your lab report. Write the final net ionic
equations under Reactions M to P in the Reactions section of your lab report, or write NR for any
mixture that did not form a precipitate. Save all solutions in the waste beaker on your lab bench
and clean the four test tubes. Dispose of the contents of the waste beaker in the Liquid Waste bottle
in Fume Hood A.

6. Clean and wipe dry your laboratory work area and all apparatus. When you have completed
your lab report have the instructor inspect your working area. Once you’re working area has been
checked your lab report can then be turned in to the instructor.
Post lab. Questions

 Classify the following compounds/ salts as soluble or insoluble in water.

a. CaCO3, NaCO3,AgCl, BaSO4, KNO3, MgSO4

EXPERIMENT 4: Oxidation-Reduction Reactions

Objective: to study about oxidation reduction reactions and determination of oxidizing and
reducing agents

Theory

Oxidizing agents are compounds or ions that contain an element capable of achieving a lower
oxidation state by gaining electrons. The stronger the tendency for a compound or ion to acquire
electrons, the stronger oxidizing agent it is. This experiment will look at four reactions that involve
strong oxidizing agents. Colors of various transition metal ions will aide you in predicting the
products of the oxidation-reduction reactions you will be carrying out involving metals and metal
ions. Transition metal ions with a partially filled d sublevel are usually colored, whereas ions from
non-transition metals or those with filled d sublevels are not. This is because the electron
transitions between orbital’s in ions with partially filled d sublevels absorb some of the visible
spectrum. In solution, copper (II) ions show a blue or green color. The permanganate ion in
solution shows a purple color. In solution, the dichromate ion is orange while chromium (III) ions
show a blue or green color. Iron (III) ions are yellowish-orange in solution. Metal ions without a
partially filled d sublevel, such as sodium ions, potassium ions, or zinc ions, are colorless. Colors
of various elemental halogens will aide you in predicting the products of the oxidation-reduction
reactions you will be carrying out involving halogens and halide ions. Colors of the halogens have
been seen in earlier experiments. In the nonpolar liquid hexane, bromine shows a red to light
orange color depending on its concentration, and iodine shows a violet color. The halogens
dissolve slightly in water, with bromine showing a pale brown color and iodine showing a pale
orange color.
Chemicals and apparatuses

Nitric acid, potassium permanganate, rubber stopper, delivery tube, beakers, hexane, potassium
dichromate, sodium bromide, hydrogen peroxide, iron (III)nitrate, measuring cylinder, distilled
water.

Procedure

1. Except for the laboratory handout, remove all books, purses, and such items from the
laboratory bench top, and placed them in the storage area by the front door. For laboratory
experiments you should be wearing closed-toe shoes. Tie back long hair, and do not wear
long, dangling jewelry or clothes with loose and baggy sleeves. Open you lab locker. Put
on your safety goggles, your lab coat, and gloves.
2. Reaction 1 - Nitric Acid As An Oxidizing Agent
2. Position the snorkel hood so that it is about 15 inches above the lab bench. Obtain a
one-hole rubber stopper equipped with a glass bend from the back of the lab room.
Select a test tube that fits the one-hole stopper. Under the snorkel hood support the test
tube with a clamp angle. Attach the one-hole rubberon a ring stand at a 45 stopper
equipped with a glass bend. Half fill a 400-mL beaker with water and place it under the
snorkel hood. Place the end of the glass bend in the beaker of water.

3. Disconnect the stopper from the test tube, and add the two or three pieces of copper
metal. Measure out about 5 mL of concentrated nitric acid, add it to the test tube, and
quickly reconnect the stopper.
CAUTION: Concentrated nitric acid causes severe burns. If the nitric acid spills on the
bench top or on the ring stand, neutralize it with sodium bicarbonate before cleaning it up.
3. Observe and record the color of the gas in the test tube. Name the colored gas in your
Data Table. After several minutes observe and record the color of the resulting solution
in the test tube. Name the colored chemical species in your Data Table. Disconnect the
stopper from the large test tube under the snorkel hood at your lab station to release the
poisonous gas into the hood. The water from the 400- mL beaker can be poured down
the sink. The solution in the test tube should be disposed of in the Liquid Waste bottle
in the Fume Hood A. Rinse out the glass bend and the rubber stopper with water, and
return it to the back of the lab room. Work out the balanced ionic equation in the
Reaction.
4. Reaction 2 - Permanganate As An Oxidizing Agent

5. Place 5 mL of sodium bromide solution in a medium test tube and add 2 drops of
concentrated nitric acid. Add about 20 drops of the immiscible liquid hexane, which will
form a clear layer on top of the aqueous solution of sodium bromide. The hexane is not
involved in the chemical reaction, but one of the products of the reactions readily dissolves
in it upon mixing.
6. Record the color of the potassium permanganate solution and name the colored chemical
species in your Data Table. Add ten drops of the potassium permanganate solution and mix
the contents of the test tube with the vortex mixer. Record the color in the hexane layer. If
no color is present in the hexane layer, add ten more drops of the potassium permanganate
solution, mix as before and record the color in the hexane layer. Name the colored chemical
species in your Data Table. The solution in this reaction should be disposed of in the Liquid
Waste bottle in the fume hood. Work out the balanced ionic equation in the Reaction.

5. Reaction 3 - Dichromate as an Oxidizing Agent

7. Record the color of the potassium dichromate solution and name the colored chemical
species in your Data Table. Place 20 drops of the potassium dichromate solution in a
 medium test tube and add 2 drops of concentrated nitric acid. Add 10 drops of hydrogen
peroxide solution, shake the test tube, and looking for any sign of chemical action other
than a color change. Name the product giving you the sign of chemical action your Data
Table. Add 10 drops of the hydrogen peroxide solution twice more, shaking after each
addition. Record your observations, including the final color of the solution and name the
colored chemical species in your Data Table. The solution in this reaction should be
disposed of in the Liquid Waste bottle in the fume hood. Work out the balanced ionic
equation in the Reaction.

5. Reaction 4 - Metal Ions as Oxidizing Agents

8. Record the color of the iron (III) nitrate solution and name the colored chemical species
in your Data Table. Place 20 drops of the iron (III) nitrate solution in a medium test tube.
Add 20 drops of sodium iodide solution to the same test tube.
9. Add about 20 drops of the immiscible liquid hexane, which will form a clear layer on
top of the aqueous solution. The hexane is not involved in the chemical reaction, but one
of the products of the reactions readily dissolves in it upon mixing. Mix the contents of the
test tube with the vortex mixer. Record the color in the hexane layer and name the colored
chemical species in your Data Table. The solution in this reaction should be disposed of in
the Liquid Waste bottle in the fume hood. Work out the balanced ionic equation in the
Reaction.

Post lab. Questions

1. When dilute nitric acid is used as an oxidizing agent instead of concentrated nitric acid,
nitrogen monoxide gas is produced rather than nitrogen dioxide gas. Assuming in Reaction
 1 that dilute nitric acid was used instead of concentrated nitric acid, predict the products
and write the balanced net ionic equation.
2. Assuming the reaction conditions for Reaction 2 were a basic solution instead of an
acidic solution, predict the products and write the balanced net ionic equation.

EXPERIMENT 5: Valances of Vanadium

Objective: to determine the oxidation states of vanadium

Theory

Vanadium is one of the first row transition metals in the periodic table. Its valance electronic
configuration is 4s2 3d3. Hence, its oxidation states are +II (losing 4s electrons), +III, +IV and +V
(losing all 4s and 3d electrons). Species from these different oxidation states can be recognized
from their colors.

Species oxidation state color

V2+ +II purple
V3+ +III Green
VO2+ +IV blue
VO2+, VO3+ +V yellow

Vanadium in high oxidation state is a strong oxidizing agent. For example, dioxovanadium (V)
ion, VO2+, oxidizes sulfite ion (SO32-) to sulfate ion (SO42-) in acidic solution. It is then reduced to
oxovanadium (IV) ion, VO2+.

2VO2+ + SO32- + 2H+ → 2VO2+ + SO42- + 2H2O (10)

Yellow blue

In acidic solution, dioxovanadium (V) ion, VO2+, oxidizes Zn to Zn (II). It is then reduced to V
(II).

2VO2+ + 3Zn + 8H+ → 2V2+ + 3Zn2+ +4H2O (11)

 Yellow purple
Oxovanadium (IV) ion was oxidized by permanganate ion to dioxovanadium (v) ion
2VO2+ + MnO4-+ 2H+ → 2VO2+ + Mn2+ + 2H+(12)
Blue yellow

Chemicals and apparatuses

Beaker, volumetric flask, Pipette, and conical flask, NH4VO3, NaOH, dilute sulphuric acid,
distilled water, sodium sulfide crystal, KMnO4, and zinc amalgam.

Procedures

(A) Preparation of dioxovanadium (V) ion, VO2+,oxovanadium(V) ion, VO3+, solutions

1. Dissolve about 2g of ammonium metavanadate (NH4VO3) in about 50 cm3 of sodium
hydroxide aqueous solution (1M) in a 500cm3 beaker.
2. While stirring the solution formed, add 80cm3 of dilute sulfuric acid.
3. Transfer the solution into a 250-cm3 volumetric flask and add distilled water to the
calibration mark. Shake the volumetric flask vigorously and record the color of the
solution.
(B) Reduction of dioxovanadium (V) ion, VO2+, and oxovanadium (V) ion, VO3+, to oxovanadium
(IV) ion, VO2+.
1. Pipette 25cm3 solution from (a) in to a 250-cm3 conical flask and add about 20cm3 dilute
sulfuric acid and some sodium sulfide crystal until the solution change to blue color.
2. Heat the mixture to boiling to remove all excess of sulfur dioxide gas. The presence of
the gas can be tested using a piece of filter paper dipped in dilute potassium
permanganate. (Sulfur dioxide gas will decolorize potassium permanganate).
3. Titrate the hot solution with potassium permanganate (0.02M) until the color changes
from blue to yellow.
(C) Reduction of dioxovanadium (V) ion, VO2+, and oxovanadium (V) ion, VO3+, to vanadium (II)
ion, V2+.
1. Pipette 25cm3 solution from (a) in to a clean 250-cm3 conical flask fitted with a stopper,
and add approximately 20cm3 dilute sulfuric acid.
 2. Add zinc amalgam (2%) in to the solution, close the flask and shake it vigorously until
the color turns purple.
3. Measure approximately 60cm3 solution from (a) in to a clean 500-cm3 beaker. Decant
as much as possible of the reduced solution (purple color) quickly into the beaker
containing the solution from (a). Record the color of the solution.
4. Introduce 10cm3 of dilute sulfuric acid in to the flask containing zinc amalgam and shake
vigorously, and again decant in into the 500-cm3 beaker.
5. Repeat step 4 two more times
6. Heat the solution in the 500-cm3 beaker and titrate it with potassium permanganate
(0.02M) until the color turns yellow.

Post lab. Questions

1. What is the color of dioxovanadium (V) ion?

2. Why is the ratio of the volume of KMnO4 in (a) and (b) equals 1:3?
3. Write the equations of all the Redox reactions in this experiment?

EXPERIMENT 6: Chemistry of Chromium

Objective: to study the chemistry of chromium

Theory
Chromium is the 24th element in the periodic table and it is found in about 0.0122% of the Earth's
crust. It is named after the Greek word "chroma," meaning color. This element produces many
beautifully colored compounds, as well as a wide array of colored solutions. Chromium is also a
very useful industrial metal. Chromium is a blue- gray metal that can be polished to achieve a high
shine. It is extremely lustrous and while it is relatively hard, it is also very brittle. Chromium is a
fairly active metal. While it does not react with water, it does react with most acids. It reacts with
oxygen at room temperature to form chromium (III) oxide. One of chromium's most important
properties is its self-passivation. While it is stable in air, chromium will oxidize to form a thin
layer that acts as a protective coating to prevent further corrosion.

The chemistry of chromium (principal oxidation states +3 and +6) is described with particular
emphasis on chromium (III) complex ions with ligands such as water, ammonia and chloride ion
etc. The atomic number of chromium is 24 and its electronic configuration is [Ar]
3d54s1 and not [Ar] 3d44s2. Or Cr, Z=24, 1s22s22p63s23p63d54s1

Uses of CHROMIUM

Chromium is a hard bluish–white metal that is extremely resistant to chemical attack at room
temperature e.g. very resistant to oxidation.

Chromium is used in the production of extremely hard steel alloys e.g. ball bearings.

Chromium metal is an important component in 'stainless steel'.

Chromium is used to electroplate other metals like steel because of its anti–corrosion properties
('chrome/chromium plating').

Chromium (III) oxide, Cr2O3 is used in stained glass and a catalyst in the chemical industry.

Chromium (IV) oxide is used in magnetic tapes for sound/video recording.

Extraction of chromium

Chromium ore is processed and purified into chromium(III) oxide. This is reacted, very
exothermically, in a Thermit style reaction, with aluminium (see reactions of aluminium) to free
the chromium metal.
Cr2O3(s) + 2Al(s) ==> Al2O3(s) + 2Cr(s)

The chromium (III) oxide is reduced to chromium by O loss, the aluminium is oxidised to
aluminium oxide by O gain, and the aluminium is the reducing agent i.e. the O remover.

These are examples of metal displacement reactions e.g. the less reactive chromium or titanium
are displaced by the more reactive sodium, magnesium or aluminum.

Chemicals and apparatuses:

Sodium hydroxide, Sodium carbonate / bicarbonate, ammonia solution, chromium sulphate

solution, hydrogen peroxide, test tubes, test tube racks, test tube holder, distilled water, measuring
cylinder, ammonium dichromate, KCr(SO4)2.12H2O or chromium sulphate, sulphuric acid.

Procedure

1. Preparation of chromium (|||) compound

Grinds some ammonium dichromate in mortar and place the powder in to a test tube. Clamp tube
on a stand in a vertical position and heat with a Bunsen burner. In doing so, the orange starting
compound turns in to a dark green, voluminous substance with the formula Cr2O3.

(NH4)2Cr2O7 → Cr2O3 + N2+4H2O

2. Preparation of chromic hydroxide

Take 3-4 drops of aqueous solution of KCr (SO4)2.12H2O or chromium sulphate. Both salts
contain the grayish violet [Cr (H2O) 6]3+, complex cation. Add 1-2 drops of 2N NaOH. If excess
of alkali hydroxide has been properly avoided, a grayish green, gel like precipitate of Cr (OH) 3 is
observed.

Cr3+ +3OH- → Cr (OH) 3

3. Amphoteric character of chromium (|||) hydroxide

Prepare Cr (OH)3 in two test tube as described above. Add drop wise 2N sulphuric acid in to the
first tube and 2N NaOH in to the second one. Notice the color of the resulting solutions. Write the
reaction.

Reactions of chromium (III) ions in solution

The simplest ion that chromium forms in solution is the hexaaquachromium (III) ion -
[Cr(H2O)6]3+.

The acidity of the hexaaqua ions of chromium

In common with the other 3+ ions, the hexaaquachromium (III) ion is fairly acidic - with a pH for
typical solutions in the 2 - 3 range.

The ion reacts with water molecules in the solution. A hydrogen ion is lost from one of the ligand
water molecules:

The complex ion is acting as an acid by donating a hydrogen ion to water molecules in the solution.
The water is, of course, acting as a base by accepting the hydrogen ion.

Because of the confusing presence of water from two different sources (the ligands and the
solution), it is easier to simplify this:

However, if you write it like this, remember that the hydrogen ion isn't just falling off the complex
ion. It is being pulled off by a water molecule in the solution. Whenever you write "H +(aq)" what
you really mean is a hydroxonium ion, H3O+.

4. Ligands exchange reactions involving chloride or sulphate ions

The hexaaquachromium (III) ion is a "difficult to describe" violet-blue-grey colour. However,

when it is produced during a reaction in a test tube, it is often green.
We nearly always describe the green ion as being Cr3+(aq) - implying the hexaaquachromium(III)
ion. That's actually an over-simplification.

What happens is that one or more of the ligands water molecules get replaced by a negative ion in
the solution - typically sulphate or chloride.

Replacement of the water by sulphate ions

Heat chromium (III) sulfate solution, the violet-blue chromium (III) sulfate solution turns green.

[Cr(H2O)6]3+ + heat --> [Cr(H2O)5(SO4)]4+

One of the water molecules in the complex ion is replaced by a sulfate ion.
Two positive charges are replaced by two negative charges of the sulfate ion.

Replacement of the water by chloride ions

Heat chromium (III) chloride solution; the violet-blue chromium (III) chloride solution turns
green.

[Cr(H2O)6]3+ + heat --> [Cr(H2O)4Cl2]+ green, tetraaquadichlorochromium (III) ion;

hexaaquachromium (III) ion --> tetraaquadichlorochromium (III) ion, two of the water molecules
in the complex ion are replaced by chloride ions.

5. Reactions of hexaaquachromium (III) ions with hydroxide ions

The violet-blue chromium +3 ion solutions reacts with sodium hydroxide forms a gelatinous light
blue precipitate, with excess sodium hydroxide re dissolves to form a green solution.

[Cr (H2O)6]3+ + 3OH- sodium hydroxide solution --> 3H2O + [Cr(H2O)3(OH)3] (s); a hydrogen is
removed from three of the water molecules in the complex ion to form a neutral complex
precipitate and water.
[Cr(H2O)3(OH)3] (s) + 3OH- excess sodium hydroxide solution --> [Cr(OH)6]3- + 3H2O

6. Reactions of hexaaquachromium (III) ions with ammonia solution

The ammonia acts as both a base and a ligand. The violet-blue hexaaquachromium (III) ion
solution reacts with ammonia forms a light blue precipitate. However, with excess ammonia, most
of the precipitate dissolves to form a red-blue solution.

[Cr(H2O)6]3+ + 3NH3 dilute ammonia solution, acting as a base --> [Cr(H2O)3(OH)3] + 3NH4+

A hydrogen removed from three of the water molecules in the complex ion to form a neutral
complex precipitate and ammonium ion.

[Cr(H2O)6]3+ + 4NH3 excess concentrated ammonia solution, then left to stand <-->
[Cr(NH3)6]3+ + 6H2O

Ammonia replaces water as a ligand in the complex ion to form hexaamminechromium (III) ions.
This reaction is a ligand and exchange reaction.

7. Reactions of hexaaquachromium (III) ions with carbonate ions

If you add sodium carbonate solution to a solution of hexaaquachromium (III) ions, you get exactly
the same precipitate as if you added sodium hydroxide solution or ammonia solution.

This time, it is the carbonate ions which remove hydrogen ions from the hexaaqua ion and produce
the neutral complex. Depending on the proportions of carbonate ions to hexaaqua ions, you will
get either hydrogen carbonate ions formed or carbon dioxide gas from the reaction between the
hydrogen ions and carbonate ions. The more usually quoted equation shows the Cr(III) is
precipitated by carbonate as Cr(OH)3. The precipitate is not soluble in excess carbonate.
2 [Cr(H2O)6]3+(aq) + 3 CO32−(aq) 2 [Cr(OH)3(H2O)3](s) + 3 H2O(l) + 3 CO2(g)
formation of carbon dioxide. Apart from the carbon dioxide, there is nothing new in this reaction:

8. The oxidation of chromium (III) to chromium (VI)

An excess of sodium hydroxide solution is added to a solution of the hexaaquachromium (III) ions
to produce a solution of green hexahydroxochromate (III) ions. This is then oxidized by warming
it with hydrogen peroxide solution. You eventually get a bright yellow solution containing
chromate (VI) ions.

The equation for the oxidation stage is:

[Cr(OH)6]3- + H2O2 solution + heat --> CrO42- + 2OH- + 8H2O.

Procedures

 Put about 2ml of reagent solutions of 1M ammonia, 2N Sulfuric acid, 2N sodium hydroxide
solutions, and 2N sodium carbonate solutions in to different or separate test tubes. And
then add 2-3 drops of chromium sulphate/ sulphite solution on each different test tube
containing different ligand solutions. If desired, the mixture was heated gently to increase
rate of reaction, or added in excess perhaps the precipitate formed will dissolve (especially
for Ammonia and sodium hydroxide). Note any precipitation or color changes formed
during the experiment.
 Record the color of the product and Write all the chemical reactions from the given
experiment.

Post lab. Questions

1. List different oxidation states of chromium and examples of compounds they

form.
2. What is chromium's symbol, atomic number and weight?
3. What are some common uses of chromium today?
4. What is the magnetic property of chromium?
5. Write out the electron configuration of: Cr, Cr6+, Cr2+.
6. Why is passivation an important property of chromium?
EXPERIMENT 7: The Chemistry of Iron

Objective: to study the chemistry of iron

Theory

The chemistry of iron is dominated by the +2 and +3 oxidation states i.e. iron(II) and iron(III)
complexes e.g. Fe2+ and Fe3+ complex ions with selected ligands, usually of an octahedral shape,
a few tetrahedral iron(III) complexes are mentioned too. The reactions of the aqueous ions iron(II)
and iron(III) with ammonia, sodium hydroxide and sodium carbonate are described and explained
as are complexes of iron(III) with the chloride ion and cyanide ion.

principal oxidation states of

iron, redox reactions of iron,
ligand substitution
displacement reactions of iron,
balanced equations of iron
chemistry, formula of iron complex ions, shapes colours of iron complexes, formula of compounds

Reactions of the iron ions with hydroxide ions

Hydroxide ions (from, say, sodium hydroxide solution) remove hydrogen ions from the water
ligands attached to the iron ions. When enough hydrogen ions have been removed, you are left
with a complex with no charge - a neutral complex. This is insoluble in water and a precipitate is
formed.

In the iron (II) case:

[Fe(H2O)6]2++2OH−→[Fe(H2O)4(OH)2]+2H2O

In the iron(III) case:

[Fe(H2O)6]3++3OH−→[Fe(H2O)3(OH)3]+3H2O
In the test-tube, the color changes are:

Iron is very easily oxidized under alkaline conditions. Oxygen in the air oxidizes the iron (II)
hydroxide precipitate to iron (III) hydroxide especially around the top of the tube. The darkening
of the precipitate comes from the same effect.

Reactions of Iron Ions with Ammonia

Ammonia can act as both a base and a ligand. In these cases, it simply acts as a base - removing
hydrogen ions from the aqua complex.

In the iron (II) case:

[Fe (H2O) 6]2++2NH3→ [Fe (H2O) 4(OH) 2] +2NH4+

The appearance is just the same as in when you add sodium hydroxide solution. The precipitate
again changes color as the iron (II) hydroxide complex is oxidized by the air to iron (III) hydroxide.
In the iron (III) case:

[Fe (H2O)6]3++3NH3→[Fe(H2O)3(OH)3]+3NH4+

Reactions of the iron ions with carbonate ions

There is an important difference here between the behavior of iron (II) and iron (III) ions.

Iron (II) ions and carbonate ions

You simply get a precipitate of what you can think of as iron(II) carbonate.

Fe2+(aq)+CO2−3→FeCO3(s).

Iron (III) ions and carbonate ions

The hexaaquairon (III) ion is sufficiently acidic to react with the weakly basic carbonate ion. If
sodium carbonate solution is added to a solution of hexaaquairon (III) ions, you get exactly the
same precipitate as if you added sodium hydroxide solution or ammonia solution. This time, it is
the carbonate ions which remove hydrogen ions from the hexaaqua ion and produce the neutral
complex. Depending on the proportions of carbonate ions to hexaaqua ions, you will get either
hydrogen carbonate ions formed or carbon dioxide gas from the reaction between the hydrogen
ions and carbonate ions. The more usually quoted equation shows the formation of carbon dioxide.

2[Fe (H2O) 3++3CO2−3→2 [Fe (H2O) 3(OH) 3] +3CO2+3H2O

Testing for iron (III) ions with thiocyanate ions

This provides an extremely sensitive test for iron(III) ions in solution. If you add thiocyanate ions,
SCN-, (e.g., from sodium or potassium or ammonium thiocyanate solution) to a solution containing
iron (III) ions, you get an intense blood red solution containing the ion [Fe(SCN)(H2O)5]2+.

Chemicals and apparatuses

Ammonia solution, ammonium dichromate, test tubes, test tube racks, Sodium hydroxide, test tube
holder, distilled water, measuring cylinder.

Procedures

EXPERIMENT 8: the chemistry of cobalt

Objective: to study the chemistry of cobalt

Theory

Cobalt is a transition metal of its atomic number of 27 and the electronic configuration

Co: 1s22s22p63s23p64s23d7
The chemistry of the transition metal cobalt (most common oxidation states +2 and +3) is
dominated by the stability of the cobalt(II) ion which forms a wide variety of stable complexes
with most ligands such as water, ammonia, chloride ion etc. The cobalt(III) state can be stabilised
by a suitable ligand and cobalt(III) complexes are usually made by oxidising a cobalt(II) salt in the
presence of the stabilising ligand.

Reactions of cobalt(II) ions in solution

The simplest ion that cobalt forms in solution is the pink hexaaquacobalt(II) ion - [Co(H2O)6]2+.

The reaction of hexaaquacobalt(II) ions with hydroxide ions

Hydroxide ions (from, say, sodium hydroxide solution) remove hydrogen ions from the water
ligands attached to the cobalt ion.

Once a hydrogen ion has been removed from two of the water molecules, you are left with a
complex with no charge - a neutral complex. This is insoluble in water and a precipitate is formed.

Reactions of hexaaquacobalt(II) ions with ammonia solution

The ammonia acts as both a base and a ligand. With a small amount of ammonia, hydrogen ions
are pulled off the hexaaqua ion exactly as in the hydroxide ion case to give the same neutral
complex.

That precipitate dissolves if you add an excess of ammonia. The ammonia replaces water as a
ligand to give hexaamminecobalt(II) ions.

The hexaamminecobalt(II) complex is very easily oxidised to the corresponding cobalt(III)

complex. In the test-tube this is seen as a rapid darkening to a deep red-brown solution.
In fact the hexaamminecobalt(III) ion is yellow! What you see is a mixture of this ion and various
other cobalt(III) ions involving ligand exchange reactions with both water molecules and negative
ions present in the solution.

Another oxidation of hexaaquacobalt (II) ions

Rather than relying on oxidation by the air, you can add an oxidizing agent such as hydrogen
peroxide. You can do this after the addition of ammonia as in the last case, or you can do it
following addition of sodium hydroxide solution.

With ammonia solution and hydrogen peroxide

The reaction with ammonia solution followed by hydrogen peroxide produces the same dark
reddish-brown solution as before - only faster. The equation for the oxidation of the ammine
complex is:

With sodium hydroxide solution and hydrogen peroxide

You get the variably colored precipitate of the cobalt(II) hydroxide complex when you add the
sodium hydroxide solution.

Addition of hydrogen peroxide produces lots of bubbles of oxygen and a dark chocolate brown
precipitate. The final precipitate contains cobalt in the +3 oxidation state. I haven't given a formula
for this, because I don't know exactly what it is! I can't give an equation for the same reason. The
reaction of hexaaquacobalt (II) ions with carbonate ions

You simply get a precipitate of what you can think of as cobalt (II) carbonate.

A ligand exchange reaction involving chloride ions

If you add concentrated hydrochloric acid to a solution containing hexaaquacobalt(II) ions, the
solution turns from its original pink colour to a rich blue. The six water molecules are replaced by
four chloride ions. The reaction taking place is reversible.

If you add water to the blue solution, it returns to the pink colour.

Chemicals and apparatus

Cobalt(||)salt solution,Co(OH)2 , HCl solution, NaOH solution ,[Co(OH)4]2-, hydrogenperoxide,

test tubes, test tube racks, test tube holder, distilled water, measuring cylinder.

Procedures
6. reaction of cobalt(||) with alkali hydroxide
Slowely add a few drops of concentrated aqueous sodium hydroxide to 5 drops of the Co
(||) salt solution. At a room temperature a light blue precipitate of basic salt of varying
composition is obtained. on boiling the precipitate changes to pink due to formation of
cobalt hydroxide. Write the equation.
i. solubility of Co(||) hydroxide
Prepare cobalt (||) hydroxide according to the previous experiment. To one sample add a
few drops of 2N HCl and treat another sample with an excess of concentrated NaOH. The
hydroxide dissolves readily in acid but only partly in alkali hydroxide forming the deep
blue [Co (OH) 4]2-. Write the equation.
ii. reaction of Co(||) with ammonia
Place 5 drops of the cobalt (||) salt solution in to a test tube and add drop wise dilute
ammonia solution. A blue precipitate of basic cobalt(||) salt can be observed.in the presence
of air the precipitate turns to pink and dissolves in excess ammonia. Oxidation to cobalt (||)
takes place. The resulting ammine cobalt (||) complexes are very stable. Write the equation.
iii. reactions of cobalt (||) with sodium carbonate
 Place 5 drops of the cobalt (||) salt solution in to attest tube and add an excess of sodium
carbonate solution. Depending on the concentration, a bluish or reddish precipitate of basic
cobalt carbonate is obtained. Compare with expt 1 and 2.
iv. Reaction of cobalt (||) with ammonium sulphide
Place 5 drops of cobalt (||) salt solution in to a test tube and add a few drops of aqueous
ammonium sulfide. Black cobalt sulfide is precipitated. Write the equation.
iv. oxidation of cobalt (||) hydroxide with hydrogen peroxide
Precipitate cobalt (||) hydroxide according to experiment one. Then add three drops of 6%
hydrogen peroxide and boil. Observe the formation of black solid cobalt(||) hydroxide.
Write the equation.

Post lab. Questions

1. Discuss the preparation of metallic cobalt.
2. Describe the oxides and hydroxides of cobalt and account for their behavior with
respect to acids and bases respectively.

EXPERIMENT 9: the chemistry of nickel

Objective: to study the chemistry of nickel

Theory

Nickel is the earth's 22nd most abundant element and the 7th most abundant transition metal. It is a
silver white crystalline metal that occurs in meteors or combined with other elements in ores. The
atomic number of nickel is 28 and its electronic configuration is 1s22s22p63s23p64s23d8.

Properties

Nickel is a hard silver white metal, which occurs as cubic crystals. It is malleable, ductile and has
superior strength and corrosion resistance. The metal is a fair conductor of heat and electricity and
exhibits magnetic properties below 345°C. Five isotopes of nickel are known.
In its metallic form nickel is chemically unreactive. It is insoluble in cold and hot water and
ammonia and is unaffected by concentrated nitric acid and alkalis. It is however soluble in dilute
nitric acid and sparingly soluble in dilute hydrochloric and sulfuric acids. The primary use of nickel
is in the preparation of alloys such as stainless steel, which accounts for approximately 67% of all
nickel used in manufacture. The greatest application of stainless steel is in the manufacturing of
kitchen sinks but it has numerous other uses as well. Other nickel alloys also have important
applications. An alloy of nickel and copper for example is a component of the tubing used in the
desalination of sea water. Nickel steel is used in the manufacture of armor plates and burglar proof
vaults. Nickel alloys are especially valued for their strength, resistance to corrosion and in the case
of stainless steel for example, esthetic value.

Electroplating is another major use of the metal. Nickel plating is used in protective coating of
other metals. In wire form, nickel is used in pins, staples, jewelry and surgical wire. Finely divided
nickel catalyzes the hydrogenation of vegetable oils. Nickel is also used in the coloring of glass to
which it gives a green hue.

Other applications of nickel include:

1. Coinage
2. Transportation and construction
3. Petroleum industry
4. Machinery and household appliances
5. Chemical industry.

Nickel compounds also have useful applications. Ceramics, paints and dyes, electroplating and
preparation of other nickel compounds are all applications of these compounds. Nickel oxide for
example is used in porcelain painting and in electrodes for fuel cells. Nickel acetate is used as a
mordant in the textiles industry. Nickel carbonate finds use in ceramic colors and glazes.

Uses of NICKEL

 Nickel is a moderately hard silvery–white metal, lustrous like most transition metals and
malleable and ductile.
  Nickel is quite resistant to corrosion and not affected by water but will dissolve slowly in
most strong acids.
 Nickel has many uses from 'silver' coinage metals like cupro–nickel, which is an alloy of
nickel and copper that doesn't readily corrode.
 Along with chromium, nickel is used in stainless steels.
 Alnico alloy (Al + Ni + Co) is used to make permanent magnets.
 Nichrome wire (Ni + Cr) is used to make wire for windings in electric motors.
 Nickel is a constituent of monel metal alloy used to make ships propeller shafts and
chemical reactor vessels because of its strength and anti–corrosion properties.
 Nickel is an important hydrogenation catalyst in converting unsaturated vegetable oils to
saturated fats like margarine.
o unsaturated oil + hydrogen ==> low melting solid more saturated fat
o Along the carbon chain of the vegetable oil you get: –CH=CH– + H2 ==> –CH2–
CH2–
 Solutions of nickel (II) salts or complexes are used in electroplating nickel onto other metal
surfaces.
o e.g. the complex ion salt Ni(NH4)2(SO4)2.6H2O
 Nickel (II) oxide, NiO, is used in pigments.

The chemistry of nickel is dominated by the +2 oxidation state with many nickel(II) complexes
known.

28Ni – 1s22s22p63s23p63d84s2 [Ar]3d82S2

Chemicals and apparatuses

Procedures

1.Reaction of nickel (||) with alkali hydroxide

 place 5 drops of nickel (||) salt solution in to a test tube and drop wise 2n of NaoH.
Observe the green precipitate of Ni(OH)2. The hydroxide is insoluble in excess sodium
hydroxide. Save the precipitate for the following experiment. Write down the equation.

2.oxidation of Ni(||)hydroxide by potassium peroxodisulphate

Take nickel (||) hydroxide precipitate prepared in the previous experiment, boil it and
add some crystals of solid potassium peroxodisulphate. Observe the formation of black
hydro nickel (|||) oxide. Write down the equation.

3. Oxidation of nickel (||) hydroxide by chlorine

Prepare a sample of Ni(OH)2 as done in experiment 1.then add some drops of fresh chlorine water.
The black precipitate to be observed is identical with the one in the previous experiment .write
down the equation.

4 reaction of Ni (||) with aqueous ammonia

Place 0.5ml on Ni (||) salt solution in to a test tube and ammonia drop wise. At first green Ni(OH)2
is precipitated .with excess ammonia the hydroxide is dissolved again under the formation of
hexamine complex ,[Ni(NH3)6]2+. Write the equation

Post lab questions

1. how does nickel react aqueous HCl and HNO3, respectively

2. Discuss the reaction of Ni(||) with cyanide, thiocyanate, and
dimethylglyoxime.
3. Find some simple reactions to distinguish between Ni (||), Co (||), Fe (||), and
Mn (||).
4. How is it possible to stabilize high and low oxidation states of an element?
Take nickel as an example.

EXPERIMENT 10: The Chemistry of Copper

Objective: to study the chemistry of copper

Theory
The simplest ion that copper forms in solution is the typical blue hexaaquacopper (II) ion -
[Cu(H2O)6]2+.The reaction of hexaaquacopper(II) ions with hydroxide ions

Hydroxide ions (from, say, sodium hydroxide solution) remove hydrogen ions from the water
ligands attached to the copper ion.

Once a hydrogen ion has been removed from two of the water molecules, you are left with a
complex with no charge - a neutral complex. This is insoluble in water and a precipitate is formed.

Reactions of hexaaquacopper (II) ions with ammonia solution

The ammonia acts as both a base and a ligand. With a small amount of ammonia, hydrogen ions
are pulled off the hexaaqua ion exactly as in the hydroxide ion case to give the same neutral
complex.

That precipitate dissolves if you add an excess of ammonia.

The ammonia replaces water as a ligand to give tetraamminediaquacopper (II) ions. Notice that
only 4 of the 6 water molecules are replaced.

The reaction of hexaaquacopper (II) ions with carbonate ions

You simply get a precipitate of what you can think of as copper(II) carbonate.

A ligand exchange reaction involving chloride ions

If you add concentrated hydrochloric acid to a solution containing hexaaquacopper (II) ions, the
six water molecules are replaced by four chloride ions.

The reaction taking place is reversible.

Because the reaction is reversible, you get a mixture of colours due to both of the complex ions.

You may find the color of the tetrachlorocuprate (II) ion variously described as olive-green or
yellow. If you add water to the green solution, it returns to the blue color.

Chemicals and apparatus test tubes, test tube holder, test tube racker, measuring cylinder, dropper,
copper sulphate solution, ammonia solution, hydrogen chloride or bromide, sodium nitrite, EDTA.

Procedure

 Prepare 0.25MCuSO4 solution.

 Prepare and pour the ligands of ammonia, EDTA, HBr/ HCl, and NaNO2 solutions in to
different or separate test tubes. And then add Cu2+ solution on those different test tubes
containing different ligand solutions step by step.
 Observe and record the color of the complex.
 Write all the chemical reactions from the given experiment.

EXPERIMENT 11: Synthesis of a Coordination Compound:

Objectives • Synthesize tris(ethylenediamine) nickel(II) chloride

• Practice writing balanced equations

• Apply stoichiometric principles to a chemical reaction
• Use balanced equations to predict products in chemical reactions
• Learn to identify the limiting reagent in a chemical reaction
• Calculate the theoretical yield and percent yield in a chemical reaction

Theory

Nickel (II) chloride (or just nickel chloride), is the chemical compound NiCl2.
The anhydroussalt is yellow, but the more familiar hydrate NiCl2·6H2O is green. Nickel(II)
chloride, in various forms, is the most important source of nickel for chemical synthesis. The nickel
chlorides are deliquescent, absorbing moisture from the air to form a solution. Nickel salts have
been shown to be carcinogenic to the lungs and nasal passages, in cases of long-term inhalation
exposure. Most of the reactions ascribed to "nickel chloride" involve the hexahydrate, although
specialized reactions require the anhydrous form.

Reactions starting from NiCl2·6H2O can be used to form a variety of

nickel coordination complexes because the H 2O ligands are rapidly displaced
by ammonia, amines, thioethers, thiolates, and organophosphines. In some derivatives, the
chloride remains within the coordination sphere, whereas chloride is displaced with highly basic
ligands.

Coordination compounds form when transition metals bond with a small molecule (e.g., H2O,
NH3 or CO3 2- ). When small molecules surround a larger metal atom in this fashion they are
called ligands. Transition metals occupy the central portion of the periodic table and share the
characteristic of having partially filled d orbitals. There are five different d orbitals, and the
degeneracy of the energy levels is removed when transition metals form complexes with ligands.
The energy difference between d orbitals in transition metal complexes is similar to the energy of
photons in visible light. Many coordination compounds are therefore brightly colored because
some of the photons from white light are adsorbed by d electrons, resulting in transmitted light
that makes the complex appear colored. White light is composed of blue, green, and red photons.
A spectrum of the NiCl2·6H2O complex (the starting material for today’s experiment) reveals that
the nickel adsorbs blue and red photons, and solutions of this nickel material appear green.
Replacing the water molecules in NiCl2·6H2O with ammonia (NH3) changes the d orbital energy
level for the central Ni2+ ion, causing solutions of the ammonium complex to adsorb green light,
transmitting red and blue light. Ammonium complexes of Ni2+ are violet for this reason. Figure
1. Hexaaquo nickel (II) ion (green) and hexaammonium nickel (II) ion (violet) Ligands form a
coordinate-covalent bond with nickel, where a non-bonded electron pair on the ligand donates two
electrons to an empty orbital on the central nickel ion. The non-bonded electron pair comes from
oxygen when the ligand is water and the non-bonded electron pair comes from nitrogen when the
ligand is ammonia. The ligand used in today’s experiment is ethylenediamine which also forms
coordinate-covalent bonds with transition metals. One molecule of ethylenediamine contains two
nitrogen atoms with non-bonded electron pairs. Therefore, only three ethylenediamine molecules
are needed to fill the six available coordination sites on Ni2+. Figure 2 shows the structure of the
ammonia and ethylenediamine molecules. ammonia ethylenediamine Figure 2.Structures of the
ammonia molecule and the ethylenediamine molecule. Note that ethylenediamine contains two
nitrogen atoms and will bond twice to a transition metal. 3 © 2015 James Madison University and
JMU Board of Visitors

Chemicals and apparatus :

NiCl2·6H2O, beaker, ethylenediamine, acetone,test tube,test tube holder,

Procedure
1. Weigh approximately 1.2 g of NiCl2·6H2O into a 100 mL beaker (Record the exact
mass).
2. Add 5 mL of deionized water, and stir to dissolve the NiCl2·6H2O
3. Add approximately 8 mL of 4.0 M ethylenediamine to the beaker (Record the exact
volume used) and stir well.
4. Add 30 mL of acetone in 10 mL increments, stirring after each addition (The product
should precipitate out of solution).
5. Cool the beaker in an ice bath to maximize precipitation, and try scratching the wall of
the beaker to initiate precipitation.
6. Vacuum filter the product. Wash with acetone. DO NOT USE WATER-the product is
water-soluble and your product will be lost if you add water. NOTE: Remember to pre-
weigh petri dish AND filter paper.
7. Dry under vacuum filter until product is crystalline (4-5 minutes).
8. Transfer the product and filter paper to a pre-weighed petri dish and air dry the product
for 5 minutes in the fume hood.
9. Dry in oven at ~60 o C for 10 minutes or until product is completely dry.
10. Allow the petri dish to cool and then weigh the petri dish, product, and filter paper.
11. Deposit the product in the waste container labeled "Solid
tris(ethylenediamine)nickel(II) chloride."

Data Table
Mass NiCl2·6H2O (g) __________________________
Color __________________________
Volume NH2CH2CH2NH2 (mL) __________________________
Concentration of NH2CH2CH2NH2 (mol/L) __________________________
Mass Ni(NH2CH2CH2NH2)3Cl2 + petri dish + filter paper (g)
__________________________ Mass petri dish + filter paper (g)
__________________________
Mass Ni(NH2CH2CH2NH2)3Cl2 (g) __________________________
Color __________________________
Results Table
Moles NiCl2·6H2O used __________________________
Moles NH2CH2CH2NH2 used __________________________
Moles Ni(NH2CH2CH2NH2)3Cl2 produced __________________________
Limiting reagent __________________________
Theoretical yield (based on the limiting reagent) (g) __________________________
Actual yield (g) __________________________
% Yield

EXPERIMENT 12: Synthesis of Tris(ethylenediamine)cobalt(lll) chloride

Objective: to synthesize Tris(ethylenediamine)cobalt(lll) chloride as a coordination
compound

Theory
Tris(ethylenediamine)cobalt(III) chloride is a coordination complex with the formula
[Co(en)3]Cl3 (where "en" is the abbreviation for ethylenediamine ).
This complex was important in the history of coordination chemistry because of its
stability and its stereochemistry. Many different salts have been described. The complex
was first described by Alfred Werner who isolated this salt as yellow-gold needle-like
crystals.[1] The compound is prepared from an aqueous solution of ethylenediamine and
virtually any cobalt(II) salt, such as cobalt(II) chloride. The solution is purged with air to
oxidize the cobalt(II)-ethylenediamine complexes to cobalt(III). The reaction proceeds in
95% yield, and the trication can be isolated with a variety of anions. A detailed product
analysis of a large-scale synthesis revealed that one minor by-product was
[Co(en)2Cl(H2NCH2CH2NH3)]Cl3, which contains a rare monodentate ethylenediamine
ligand (protonated).[
Chemical: CoCl2.6H20, H202, HCI, ethylenediamine, anhydrousethylanediamine,
ethanol,
Apparatus:

Procedure
dissolve 12.0 g CoCl2.6H20 in 35 ml water; while this is dissolving add 9.0ml of anhydrou
sethylanediamine to 25 ml water,cool in ice and add 8.5 ml 6N HCI. Add the CoCl2
solution to the partially neutralized ethylenediamine and then add 10 ml of 3O%H202 with
stirring. Stir for a few minutes until effervescence ceases, place the mixture on a hot plate
and boil gently. When the solution has evaporated to a volume of 60 ml, an equal volume
of conc. hydrochloric acid is added followed by 120 ml ethanol. Cool in ice and filter,
washing with two portions of ethanol and two portions of ether. Air dry.
Results. Following this procedure students obtain approximately 10 g of the complex;
evaporation to lower volumes does not afford significant improvement while evaporation
to very low volume (20-30 ml) gives a large amount of a green impurity. During the
evaporation we have students synthesize tris(ethylenediamine)nickel(II) chloride. They
can then compare the two (e.g., lability in acid). '