SKT3013: Inorganic Chemistry I

LABORATORY MANUAL

SKT 3013
INORGANIC CHEMISTRY I

Department of Chemistry
Faculty of Science and Mathematics
UNIVERSITI PENDIDIKAN SULTAN IDRIS

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SKT3013: Inorganic Chemistry I

No Experiment Pages

0 Safety Rules and Regulations in Chemistry Laboratory 3

1 Crystallization of Impure Acetanilide 7

2 Gravimetric Analysis of Tin Alloy 14

3 Inorganic Qualitative Analysis 17

4 Molecular Formula Determination of Hydrazinium Sulphate 21

5 Molecular Symmetry 24

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SKT3013: Inorganic Chemistry I

SAFETY RULES AND REGULATIONS IN CHEMISTRY LABORATORY

1. DO NOT ENTER the laboratory without the permission of the laboratory instructor.
2. All bags should be placed on the rack provided. All gadgets (handphone, tablet, etc) are
NOT ALLOWED during experiments.
3. Please wear a proper attire to work in the lab (Short pants, short skirt, “purdah”,
sleeveless shirt are not permitted).
4. Wearing jewellery is not permitted in the laboratory.
5. Long hair and scarf must be properly manageable.
6. DO NOT wear contact lenses.
7. Wearing personal protection equipment (PPE) is compulsory in laboratory such as lab
coat, cover shoes and safety glasses, gloves and etc.
8. Student are NOT ALLOWED to smoke, drink, eat, play around and run in laboratory
9. Know the location of all safety equipment.
10. No experiment can be performed without the permission of the laboratory instructor.
11. Read the label on the container of a chemical twice to make sure you are using the right
chemicals. Follow the instructions properly. DO NOT waste chemicals. Use required
amount only.
12. DO NOT contaminate chemicals. Once chemical has been removed from their containers,
DO NOT put it back into the stock container.
13. DO NOT use cracked or chipped glassware.
14. NEVER use mouth suction when using a pipette. Use a pipette filler/bulb.
15. DO NOT leave any heating, vigorous or rapid reaction unattended.
16. Always use fume hood when working with flammable organic compounds, strong acid and
base, volatile solvent, corrosive and toxic materials.
17. DO NOT heat flammable materials directly.
18. Make sure your surrounding is safe before using Bunsen burner.
19. While heating chemicals in test tubes, NEVER point the tubes to yourself or others.
20. Waste chemicals must be disposed properly by placing them in waste container provided.
Ask your instructor how to discard used reagents.
21. Broken apparatus, water and gas leakage must be reported to laboratory assistant on duty
immediately.
22. In case on fire or hearing emergency siren, evacuate the laboratory quickly in orderly
manner. In case of small accident or small fire occurs, try to overcome them wisely.

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23. Report any accidents (minor or major) to your laboratory instructor. This accident must be
recorded in log book “CATATAN KEMALANGAN”.
24. Clean all glassware and place them appropriately before leaving laboratory. Make sure to
switch off instruments, water and gas supplies.
25. Final year project students should require permission from supervisor and head of
department if they want to work after normal working hours.

AN EXPERIMENT DONE WELL IS......

AN EXPERIMENT DONE SAFELY

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SKT3013: Inorganic Chemistry I

GUIDELINE TO WRITE LAB REPORT

OBJECTIVE
State the objective clearly in a complete sentence. A few explanatory sentences may be included,
if needed.
The objective should answer the question: What is the lab objective designed to determine?

EXPERIMENTAL PROCEDURE
The experimental methods should give a detailed description in your own words of how YOU
accomplished the experimentation (Passive voice sentences).
*Tips: This should include equipment used in the experiment as well as how it was used. The
description should have sufficient detail so that another experimenter could duplicate your efforts.
Use sketches and diagrams to describe the experimental set-up. Label the main components.
Tips: Any information copied directly from Lab manuals or other references should be stated
within quotes and referred, otherwise, it is considered plagiarism.

RESULTS AND DISCUSSION

This is the most important part of the report. Summarize your results in the introductory sentence.
Relate your results to your objective. Present the results in the easiest way for your reader to
understand: graphs, tables, figures, etc.
Spreadsheets are often an ideal tool for organizing the data, analyzing the data, and generating
graphs and tables. All tables and figures should be accompanied by comments or discussions in
the text of report; use a numbering system for identification of each one.
All figures and tables must have numbers and captions. While the table captions should be placed
over the table, figure captions should be placed below the figure.
Explain the results of the experiment, comment on the results you obtained, compare obtained
results with expected results, give probable reasons for discrepancies from the correct results,
answer any questions outlined in the instructions and solve any problems that may have been
presented. Tell why things happened, not only that they did happen. Implementation errors
should be discussed here.

CONCLUSIONS
State your discoveries, judgments and opinions from the results of this experiment and relate it
with your experiment objectives. Suggest ways to improve the results of this experiment.
REFERENCES

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List the book, publication or website that you referenced in writing your report. Provide authors,
publisher, date of publication, page number, etc.
*Tips: Follow the standard format for typing a reference:
[1] Little, P., and Cardenas, M., “Use of Studio Methods in the Introductory Engineering Design
Curriculum,” Journal of Engineering Education, Vol. 90, No. 3, 2001, pp. 309-318.
[2] Nunally, J., Psychometric Theory, 2nd ed., New York, N.Y.: McGraw-Hill, 1978.
[3] Lister, B., “Next Generation Studio: A New Model for Interactive Learning,”
www.ciue.rpi.edu/pdfs/nextGenStudio.pdf.

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SKT3013: Inorganic Chemistry I

EXPERIMENT 1
CRYSTALLIZATION OF IMPURE ACETANILIDE

1.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. understand the basis of purifying organic solid compound
2. know that recrystallization is one of the techniques to purify the organic solid compound

1.2 INTRODUCTION
The principle behind recrystallization is that the amount of solute that can be dissolved by a
solvent increases with temperature. In recrystallization, a solution is created by dissolving a solute
in a solvent at or near its boiling point. At this high temperature, the solute has a greatly increased
solubility in the solvent, so a much smaller quantity of hot solvent is needed than when the solvent
is at room temperature. When the solution is later cooled, after filtering out insoluble impurities,
the amount of solute that remains dissolved drops precipitously. At the cooler temperature, the
solution is saturated at a much lower concentration of solute. The solute that can no longer be
held in solution forms purified crystals of solute, which can later be collected. Recrystallization
works only when the proper solvent is used. The solute must be relatively insoluble in the solvent
at room temperature, but much more soluble in the solvent at higher temperature (Table 1.1). At
the same time, impurities that are present must either be soluble in the solvent at room
temperature or insoluble in the solvent at a high temperature.

Table 1.1: List of solutes and solvents with different temperature

Solute Solvent Temperature (°C) Solubility (g/100 ml)
Acetanide Ethanol 20 25.0
60 257.0
Acetanilide Water 25 0.56
100 5.0
Benzoic Water 18 0.27
acid 75 2.2
Cholesterol Ethanol 17 1.0
78 11.0
Iodoform Ethanol 18 1.3
78 7.3
Succinic Water 20 6.8
acid 100 121.0

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Seven Major Steps in the Recrystallization Process:

i. Choose specific and proper solvent

If the solvent is not specified, you will need to test a variety of solvents to determine what will work
best for the solute you are trying to recrystallize. This testing can be accomplished by putting a
small amount of your solute (about the size of a pea) into three small test tubes. In each test tube,
place 0.5 ml of each potential solvent. Use a stirring rod to agitate the solute or "flick" the bottom
of the test tube with one finger while holding the top with the other hand.
If no solvent can be found, perhaps you will need to use a mixed solvent. If two solvents in which
the solute has different solubility characteristics are mixed, sometimes an appropriate solvent can
be found. For instance, if your solute is insoluble in water, but soluble in ethanol at room
temperature, a mixture of the two solvents may produce an appropriate solvent in which the solute
is insoluble at room temperature but very soluble at a significantly higher temperature.
To find the proper proportion of water to ethanol in this example, first, completely dissolve your
solute in ethanol at room temperature. Then, begin to add water until the solution becomes cloudy
(this is because all of the solute is no longer held in solution). Add just enough ethanol to make
your solution clear and begin your recrystallization procedure.
In general, a very polar solute will easily be dissolved in a polar solvent and will be fairly insoluble
in a non-polar solvent. Frequently, having a solvent with slightly different polarity characteristics
than the solute has been better because if the polarity of the two is too closely matched, the solute
will likely be at least partially dissolved at room temperature.
Some commonly used solvents: water, methanol, ethanol, acetone, ethyl acetate, chloroform,
carbon tetrachloride, benzene, hexane and petroleum ether.

ii. Dissolving the impure solute in the hot solvent

Add a small portion of boiling solvent to the beaker that contains the impure sample and a boiling
chip.
Heat the beaker containing the solute and continue adding boiling solvent incrementally until all
of the solute has been dissolved. If additional solvent can be added with no appreciable change
in the amount of solute present, the particulate matter is probably insoluble impurities.

iii. Remove the insoluble impurities

Gravity filtration is the method to remove solid impurities from an organic liquid. The "impurity"
can be a drying agent or an undesired side product or leftover reactant. A filtration procedure
called "hot gravity filtration" is used to separate insoluble impurities from a hot solution. Hot
filtrations require fluted filter paper (Figure 1.1) and careful attention to the procedure to keep the

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apparatus warm, but covered so that solvent does not evaporate. This fluted filter paper will give
a maximum filtration surface, also give a minimum cooling and forming of crystals on the glass
funnel-fluted filter paper.

Figure 1.1: Diagram of how to fold fluted filter paper

Filtering funnel:
- Stem funnels: used for gravity filtration. They are also used for miscellaneous tasks such
as filling round bottom flasks with liquids.
- Stem less funnel: designed for "hot filtrations". This procedure is used to filter a hot solution
of a compound in a recrystallization process; the "no-stem" feature prevents the compound from
crystallizing out too soon, e.g., in the stem of the funnel.

iv. Decolorizing solution

If the impure compound contains traces of colored material that are not native to the compound,
they may be removed by adding a small amount of decolorizing charcoal to the hot solution.

v. Formation of crystals
- Slow cooling of a hot, saturated and filtered solution to room temperature
Cooling the solution with an ice only is used until crystals begin to form. After they do, the solution
should be allowed to warm to room temperature so crystal formation occurs more slowly.
Take a fire polished stirring rod and etch (scratch) the glass of your beaker. The small pieces of
glass that are etched off of the beaker serve as nuclei for crystal formation.
- Adding a single crystal of pure material (a seed crystal).
Take a small amount of your solution and spread it on a watch glass. After the solvent evaporates,
the crystals that are left behind can serve as seeds for further crystallization. Both these methods

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of nucleation (i.e. etching and seed crystals) cause very rapid crystallization, which can lead to
the formation of impure crystals.
Heating the solution for a period of time in order to evaporate some solvent. The new,
concentrated solution, should be cooled to stimulate the recrystallization of product.

vi. Obtaining crystals of the solute

Vacuum filtration is used primarily to collect a desired solid, for instance, the collection of crystals
in a recrystallization procedure. Vacuum filtration uses either a Buchner or a Hirsch funnels
(Figure 1.2). Vacuum filtration is faster than gravity filtration, because the solvent or solution and
air are forced through the filter paper by the application of reduced pressure. If you DO NOT need
the filtrate, but only need the solid matter collected on the Buchner funnel.

Figure 1.2: Diagram of vacuum filtration

vii. Purity determination

The purity of the sample can be measured by performing a melting point determination.
If you want to use the melting point to identify a solid compound which you have isolated in the
lab, you will need to compare its melting point with that of the true compound.
Pure, crystalline solids have a characteristic melting point, the temperature at which the solid
melts to become a liquid. The transition between the solid and the liquid is so sharp for small
samples of a pure substance that melting points can be measured to ± 0.1oC.
A pure substance generally has a melting range (the difference between the temperature where
the sample starts to melt and the temperature where melting is complete) of one or two degrees.
Impurities tend to depress and broaden the melting range so the purified sample should have a
higher and smaller melting range than the original, impure sample.
To prepare a solid sample for a melting point determination press the open end of a melting-point
capillary tube down onto the sample so that the sample is forced up into the tube. Turn the tube
right-side up and tap it on the lab bench to knock the sample down to the closed end. Dropping
the capillary inside a long piece of glass tubing is effective for this step.

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Characterization of material using FTIR

FT-IR stands for Fourier Transform Infra Red, the preferred method of infrared spectroscopy. In
infrared spectroscopy, IR radiation is passed through a sample. Some of the infrared radiation is
absorbed by the sample and some of it is passed through (transmitted). The resulting spectrum
represents the molecular absorption and transmission, creating a molecular fingerprint of the
sample. Like a fingerprint no two unique molecular structures produce the same infrared
spectrum. This makes infrared spectroscopy useful for several types of analysis. FT-IR spectrum
will provide
• identity of unknown materials
• quality or consisting of a sample
• amount of components in a mixture

Chemicals
Acetanilide
Charcoal or activated carbon

Apparatus
Erlenmeyer flasks, 250 ml
Hot plate
Stem less filter funnel and fluted filter paper
Beaker, 50 ml
Buchner funnel
Rubber adaptor or stopper
Side arm filtering flask
Vacuum source
Watch glass

1.3 PROCEDURE
1. Accurately weigh out 3.0 g of impure acetanilide and put it in the Erlenmeyer flask 250
ml (A). Observe the physical appearance of that crystal. Fill a capillary tube with crystals
about 3 mm high and determine its melting point. (Note: Your instructor will demonstrate
this method).
2. Add the material to about 40 ml of distilled water.
3. Place the flask on a hot plate and slowly heat the contents to boiling. Stir the contents
occasionally.
4. When the solvent starts to boil add 5 ml of water until you cannot detect any further
disappearance of the solute. Keeps the solution boiling.

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5. Cool the solution slightly and add a small amount of decolorizing charcoal or activated
carbon. Reheat to boiling. (Note: Do not add the carbon to the hot solution. It may boil
over when the carbon is added)
6. At this period, heat another beaker containing 20 ml of distilled water to boiling.
7. Flute a piece of filter paper and place it inside of a stem less funnel. (Note: A funnel with
a stem is prone to premature recrystallization inside the stem because the filtrate can
cool as it passes through the stem)
8. Place the stem less funnel and fluted filter paper directly in the Erlenmeyer flask 250 ml
(B). Wet the filter paper using a small amount of hot distilled water so that the rising
vapours from the boiling solvent can heat the funnel and filter paper. (Note: Having the
set up heated before filtration will prevent crystals from forming on the paper and in the
funnel).
9. Pour the solution from flask A to flask B immediately through the funnel and filter paper
assembly.
10. Rinse the flask A with 10 ml of hot distilled water and pour it again through the funnel
and filter paper assembly.
11. After collecting the filtrate, pass a small amount of the hot distilled water through the filter
paper to wash the residue.
12. Set the flask aside to cool slowly to room temperature (about 15 minutes) and then chill
it in an ice bath (about 15 minutes) to induce crystallization. Then collect the crystals
using a vacuum filter apparatus.
13. Select a Buchner funnel of appropriate size for the amount of residue you are collecting,
not the amount of filtrate. Put a piece of filter paper in the funnel that fits exactly and wet
the paper using a small amount of solvent which is distilled water. (Note: Your instructor
will demonstrate this setup. Get the mass of free filter paper)
14. You are now ready to filter the solution to isolate the crystals. Swirl the flask to suspend
the crystals and then pour the slurry into the funnel.
15. Some crystals may have been left behind in the flask. An effective quantitative transfer
of all this material is by washing the crystals with a very small amount of ice cold water.
16. When the crystals have been collected and washed, allow the aspirator to run for several
minutes so that the crystals have an opportunity to dry.
17. When the crystals have been dried as much as possible in the Buchner funnel, switch off
the aspirator and take off the Buchner funnel from the vacuum source.
18. Spreading the crystals out in a beaker or a crystallizing dish will provide for the most
efficient drying as the crystals will have a maximum of exposed surface area.
19. After the crystals are dried, determine the final weight, put in the plastic bag and labelled
them. Determine the melting point of acetanilide.

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20. Determine the purity of acetanilide by comparing the FTIR spectra of impure acetanilide
with acetanilide after recrystallization.

1.4 Questions
1. Calculate the weight of pure crystal acetanilide in percentage.
2. Beside recrystallization, mention other methods that are used to purify organic
compound.
3. The desiccator is used to store dried samples in a dry atmosphere. Why it should
not be used to dry an object, for example, in this case the acetanilide?
4. Give the IUPAC name of acetanilide and one function of this compound.

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EXPERIMENT 2
GRAVIMETRIC ANALYSIS TO TIN ALLOY

2.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. understand the concept of gravimetric analysis
2. know the factors that influence the precipitation process

2.2 INTRODUCTION
Gravimetric analysis is a technique through which the amount of an analyte (the ion being
analyzed) can be determined through the measurement of mass. In order for the analysis to be
accurate, certain conditions must be met:
- The ion being analyzed must be completely precipitated.
- The precipitate must be a pure compound
- The precipitate must be easily filtered
The important method that deals with the trapping and weighing the products in the solid phase
is a precipitation method. There are two ways to bring the particles closer together and increase
the probability of coagulation and at the same time to get more precipitate:
a. Encourage digestion by heating
b. Increasing the electrolyte concentration by washing with a reagent which will go off as
a gas during the process. For instance, dilute nitric acid is effective for washing excess
ions from AgCl and the peptization process can be avoided.
During the precipitation procedure, a number of other problems can arise to give erroneous
positive or negative results. Among these are surface adsorption, mixed crystal formation,
occlusion and mechanical entrapment. In this experiment, alloy is reacts with nitric acid and
produced the precipitate of tin(IV) oxide hydrate which is metastannic acid :
3Sn + H2O + 4HNO3 3H2SnO3 + 4NO
This precipitate is heated to high temperature by using a Bunsen flame to produce tin(IV) oxide:
H2SnO3 SnO2 + H2O
The carbon from the filter paper has to be heated first at lower temperature and let the gas goes
off from the crucible. It is because the tin(IV) oxide easier, reducing to tin. Normally the colour of
the precipitate is white, but it is rare to get because the presence of some impurities.

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Chemicals
Nitric acid, concentrated
Dilute nitric acid (1%)
Tin alloy

Apparatus
Filter funnel and filter paper
Weighing bottle
Watch glass
Graduated cylinder (100 ml and 10 ml)
Beaker (150 ml and 250 ml)
Evaporating dish

2.3 PROCEDURE
1. Put enough alloy and weigh out accurately 0.15 – 0.20 g into a weighing bottle. Transfer
this alloy into a beaker, 250 ml.
(STEP 2-4 SHOULD BE HANDLED IN THE FUME HOOD)
2. Add 15 ml of concentrated nitric acid in 10 ml of distilled water. Then pour the solution
into the alloy. Put the watch glass on top of that beaker. (Always pour acids slowly into
water).
3. After the reaction burns brightly but briefly, evaporated the solution by heating it on a hot
plate until its volume becomes 5–10 ml but does not let it dries. (Note: The purpose is to
increase the particle size for easier filtering. This is usually referred to as digestion.
Digestion in this quantitative analysis refers to the coagulation of metastannic acid
precipitate into a filterable form)
4. Dilute this solution with 50 ml of distilled water and heat it again until the volume
becomes half.
5. Filter the solution into a beaker, 250 ml and make sure all the precipitate has been
transferred from the beaker to the filter. Rinse the precipitate with hot dilute nitric acid
(1%) (5 x 10 ml). Dry the precipitate in an oven to remove solvent (60°C for about 15
minutes).
6. Fold the filter paper that containing the precipitate and put it in an evaporating dish. Heat
this folded filter paper in an evaporating dish with a Bunsen flame. (Note: Your instructor
will demonstrate this method. Get the mass of the free evaporating dish)
7. Wet the precipitate with 5 drops of hot dilute nitric acid (1%). Rinse the precipitate with
distilled water for several times to remove impurities.
8. Dry the precipitate in an oven to remove solvent. After that store this dried sample in a
desiccator in a dry atmosphere. Lastly weighs the precipitate on an analytical balance.

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2.4 Questions
1. Calculation of tin in the sample (alloy) (%).
2. This gravimetric analysis does not use directly in this experiment with the presence of other
metals in the sample. Why?
3. List down some problems that can arise to give erroneous results. Determine either that
erroneous will influence the higher or lower results than the actual value.

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EXPERIMENT 3
INORGANIC QUALITATIVE ANALYSIS

3.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. understand and describe the procedures of qualitative analysis
2. know the difference between qualitative and quantitative analysis

3.2 INTRODUCTION
Unlike covalent compounds which can be identified using physical properties like boiling point
and refractive index, ionic compounds are more appropriately identified with their chemical
properties. In the qualitative analysis procedure, the chemical properties of an unknown
substance are determined by systematically reacting the unknown with a number of different
reagents. By predetermining what the particular reaction will produce if a specific ion is present,
the ions that actually are in the solution can be identified. For example, if a reaction is known to
produce a precipitate if ion A is present and a precipitate is formed when the reaction is run, then
ion A may be present in solution (there may be and usually are other ions that will also precipitate
with a particular reagent). If no precipitate is formed when the reaction is run, the ion A is clearly
not present in the unknown solution and a different reaction will have to be run to determine what
ions are present.

Chemicals
Lead(II) nitrate
Iron(II) chloride
Calcium carbonate
Calcium hydroxide solution (lime water)
Nitric acid (1 M, 3 M and 6 M)
Sodium hydroxide solution (1 M)
Ammonia solution (3 M and 6 M)
Acetic acid (6 M)
Sodium acetate (0.2 M)
Dimethylgloxime
Silver nitrate (0.1 M)
Sulfuric acid (2 M)

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Concentrated sulphuric acid

FeSO4.7H2O solid
Distilled water

Apparatus
Boiling and test tube
Graduated cylinder
Graduated cylinder
Dropper

3.3 PROCEDURE
PART A:
a. Appearance of compound
1. Identify the colour and shape of the solid iron (III) chloride (A), lead (II) nitrate (B) and
calcium carbonate (C).

b. Heating test
1. Put half spatula of solid compound in boiling tube. Heat the compound using Bunsen
burner (about 10 to 15 minutes). If a gas is given off, note the colour and odour of the
gas.
(Note: Hold the boiling tube at an angle, as shown below and point it away from yourself
and other people.)

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c. Solubility with water

1. Place half spatula of compound in 2 ml of distilled water in boiling tube and shake.
2. If the compound does not dissolve, add another 3 ml of distilled water. Shake and stir
the mixture.
3. If the compound is soluble this amount will dissolve after considerable stirring. If the
compound is moderately soluble, some of this amount will dissolve. If the compound is
insoluble, even a very small amount will not dissolve

d. Reaction with nitric acid

1. Put half spatula of solid compound in boiling tube. Add 15 ml of nitric acid (1M) to the
compound and observe any reaction that occurs (Set up the apparatus as shown below).
2. Don’t throw the mixture. Keep the solution for the reaction with sodium hydroxide and
ammonia.

e. Reaction with sodium hydroxide

1. Add 1 M of solution NaOH drop wise to the solution (used solution from test tube in
reaction with nitric acid), stir or shake the solution until precipitate form. Observe any
reactions happen.

f. Reaction with ammonia

1. Add 3 M of solution NH3 drop wise to the solution (used solution from test tube in
reaction with sodium hydroxide), stir or shake the solution and observe any reaction.
Observe any reactions happen.

PART B:
Predict the ions that present in the UNKNOWN compounds.
i. Cation Identification Test
Compound D
1. Acidify half spatula of compound D with 2 ml of acetic acid (6 M).

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2. Add 1 ml of 0.2 M of sodium acetate solution.

3. Add 1 ml of dimethylglyoxime solution and add another 1 ml drop wise. Observe any
changes colour.

Compound E
1. Acidify half spatula of compound E with 5 ml HNO3 (3 M). Test the solution with litmus
paper.
2. Add 0.1 M NH4SCN solution drop wise. Observe any changes colour.

ii. Anion Identification Test

Compound F
1. Acidify half spatula of compound F with 5 ml HNO3 (3 M) in the test tube. Test the
solution with litmus paper.
2. Pour half of the above solution in the centrifuge tube. Add several drops of 0.1 M AgNO 3
until white precipitate forms. Centrifuge and remove the supernatant.
3. Add drop wise 6 M NH3 to the precipitate with stirring until dissolved.
4. Add 6 M HNO3 to the solution until white precipitate forms.

Compound G
1. Acidify half spatula of compound G with 10 ml H2SO4 (2 M) in the boiling tube.
2. Dissolve one-half spatula full of solid FeSO4.7H2O.
3. Cool the solution with some ice for 20 minutes.

4. Add carefully 0.5 ml of concentrated H2SO4 by allowing it to flow down the side of the tilted
test tube.
5. Allow the solution to sit undisturbed for 2 hours so that the sulphuric acid forms a definite
layer.

3.4 Questions
1. Write all the balance equations for each reaction and any observations.
2. Identify the cations and anions for the unknown compounds.

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EXPERIMENT 4

MOLECULAR FORMULA DETERMINATION OF HYDRAZINIUM SULPHATE

4.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. understand the volumetric analysis that based on redox reaction to determine the
molecular formula of inorganic compound

4.2 INTRODUCTION
Hydrazine, N2H4 can produce hydrazinium salt with the same method as ammonia to produce
ammonium salt. For hydrazine, there are two types of salts that may be produced which consist
of cation [N2H5]+ or [N2H6]2+.
In this experiment we used the volumetric analysis method that based on redox reaction. The
reaction was between iodate ion, IO32- and hydrochloric acid solution. Then potassium iodate
solution which the concentration is known already was titrated with hydrazinium ion from the given
salt.
The half reaction with the electrode potential:

[IO3]- + 6H+ + 2Cl- + 4e [ICl2]- + 3H2O Eº = +1.23 V

N2 +5H+ +4e [N2H5]+
Eº = -0.23 V
N2 +6H+ +4e [N2H6]2+ Eº = -0.30 V

Write down the reactions that happened in this titration if the salts that had been produced are:
i) [N2H5]+
ii) [N2H6]2+

Determine the electrode potential for each reaction and predict the position of the reaction either
the reaction is complete or not. If the reaction is not complete then it cannot be used for further
analysis. This formula can be used to help you in predicting the reaction:
For the complete reaction, equilibrium constant, K is equal to 106 or more.

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G° = nF( E°) = -RTlnK

G° = standard free-energy change

n = number of moles electrons
F = Faraday constant
R = gas constant
T = temperature
K = equilibrium constant

lnK = [nF( E°)]

RT

Log10K = -n( E°) / 0.059 in SI unit

In the titration process:

Oxidation of iodate in HCl solution will be happened in a few steps:

[IO3]- +6H+ + 6e I- + 3H2O

[IO3]- +5I- + 6H+ 3I2 + 3H2O

[IO3]- + 2I2 + 6H+ + 10Cl- 5[ICl2]- + 3H2O

The whole equation:
[IO3]- + 6H+ + 2Cl- + 4e [ICl2]- + 3H2O

From the above equation it showed that iodine precipitated at the middle-point and disappear at
the end-point. It means that the end-point of the precipitation is where the entire hydrazinium ion
had already reacted (as indicated by disappearance of dark purple colour which is iodine colour).
To get an accurate end-point, add a little of chloroform into the solution. Iodine is more dissolve
in chloroform than in acidic water, then it will extract into chloroform layer. So you can see the
disappearance of iodine colour from the chloroform layer.
[ICl]- is not extracted to chloroform layer because it exists as an ion. This ion can dissolve in
aqueous layer which is more polar and the solution will become a pale-yellow colour
Chemicals

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SKT3013: Inorganic Chemistry I

Hydrazinium sulphate salt ([N2H5]2SO4 or [N2H6]SO4)

Chloroform
Hydrochloric acid, HCl (6.0 M)
Potassium iodate solution, KIO3 (0.025 M)

Apparatus
Graduated cylinder (50 ml)
Conical flasks / Erlenmeyer flasks, 250 ml with rubber stopper
Burette, 50 ml

4.3 PROCEDURE
1. Weigh out accurately 0.1 g of hydrazinium sulphate salt in a weighing bottle. Transfer
this salt into a conical flack, 250 ml.
2. Add 20 ml of distilled water, 30 ml of HCl (6.0 M) and 5 ml of chloroform into the flask.
Put the rubber stopper on top of that flask. (Note: Shake vigorously)
3. Using the funnel, rinse the burette with KIO3 solution (0.025 M). Fill it with the same
solution. Record the initial reading of the burette.
4. Titrate the solution in the conical flask with the KIO3 immediately until the end-point.
(Note: Colour of the chloroform layer has almost gone)
5. Use the first flask for a trial run. Record the final burette reading.
6. Repeat the titration two more times. Put your results into the results table. These
titrations should agree to within 0.10 cm3.

4.4 Questions
1. Calculate the percentage of hydrazine from the titration.
2. Determine the formula of hydrazinium sulphate that based on its percentage.
3. Draw the structure of hydrazinium ion that you get from this experiment
4. Why the hydrazine does not use as a solution?

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SKT3013: Inorganic Chemistry I

EXPERIMENT 5
MOLECULAR SYMMETRY

5.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. identify the symmetry elements and operations of the molecules or objects.
2. identify the point group of the molecules or objects.
3. determine the multiplication process of the molecules or objects.

5.2 INTRODUCTION
Molecules are classified according to their symmetry properties. Once the properties are
identified, the molecule is assigned its point group. Symmetry elements are properties which are
related to the structure of the molecule. They include mirror planes, axes of rotation, centres of
inversion and improper axes of rotation. (An improper axis of rotation is a rotation followed by a
reflection perpendicular to the rotational axis.) Symmetry operations are actions which places the
molecule in an orientation which appears to be identical to its initial orientation such as rotation,
reflection, inversion, rotation followed by reflection, and identity. The identity operation simply
leaves the molecule where it is. All molecules have the identity operation.

5.3 PROCEDURE
i. Activity 1
1. Draw the molecules or objects that have been given below.
2. Draw and write all the symmetry operations (Cn, σ, Sn, E and i) for each molecule or
object.
3. Determine the point group for each molecule or object:
a) PH3
b) [ICl4]-
c) CO2
d) CH4
e) BCl3
f) SF6
g) PF5
h) BrF5

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SKT3013: Inorganic Chemistry I

i) Beaker (50 ml) – no label

j) Test tube – no label

ii. Activity 2
1. Draw and write all the symmetry operations (Cn, σ, Sn, E and i) for each molecule or
object.
2. Determine the point group for each molecule or object.
i. Shape rectangle ii. Canadian Flag

iii. Star fish iv. KLCC tower

v. Aeroplane

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SKT3013: Inorganic Chemistry I

vi. Butterfly

vii. [Co(en)3]3+ complex viii. Organic compound

3+

5
ix. Orbital dxy x. Mg( -Cp)2

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SKT3013: Inorganic Chemistry I

iii. Activity 3
Determine either the multiplication of symmetry operation is commutative or non-commutative.
i) S3(at C3) x σh(at 2I, Fe and F) = C2(at Fe-F) x σv(at Fe,F, Br(3), Br(4))
ii) C32(at C3) x σv(at Fe,I(2), Br(3), Br(4)) = σh(at 2I, Fe and F) x C3-2(at C3)
iii) σv(at Fe,I(1), Br(3), Br(4)) x S3(at C3) = σv(at Fe,F, Br(3), Br(4)) x σh(at 2I, Fe and F)

C3
2-
r3
I2
1I e
F
r4

Bipyramidal trigon molecule [FeBr2I2F]2-

27