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DEPARTMENT OF CHEMISTRY FACULTY OF SCIENC E & MATHEMATICS UNIVERSITI PENDIDIKN SULTAN IDRIS LABORATORY MANUAL SKU3013

DEPARTMENT OF CHEMISTRY FACULTY OF SCIENCE & MATHEMATICS UNIVERSITI PENDIDIKN SULTAN IDRIS

LABORATORY MANUAL

SKU3013 CHEMISTRY I

STUDENT’S NAME

 

LECTURER’S/TUTOR’S NAME

 

MATRIC NO.

 

DATE/DAY/TIME

 

LABORATORY

 

2

SAFETY INFORMATION

CONTENTS

Experiment 1 BASIC LABORATORY TECHNIQUES

Experiment 2 DILUTION

Experiment 3 ACID AND BASE TITRATION

Experiment 4 HYDRATED SALT FORMULA

Experiment 5 CHARLES LAW

Experiment 6 DISSIMILARITY BETWEEN ELECTROVALENT AND COVALENT BOND

Experiment 7 MOLECULAR GEOMETRY

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SAFETY AND RULES IN THE CHEMISTRY LABORATORY

Student must follow the safety and rules at all times when they are working in the chemistry laboratory. This is because you are who some are harmful and hazards which must be handled in a proper manner. The following are guidelines to be followed when working in the chemistry laboratory.

  • 1. Do not enter the laboratory without the presence of the laboratory instructor.

  • 2. experiment

No

to

be

performed

without

the

permission

of

the

laboratory

instructor.

  • 3. Safety glasses must be worn at all time in the laboratory.

  • 4. Laboratory coat must be warn all times in the laboratory.

  • 5. Long hair and scarf must be properly manageable.

  • 6. Do not wear slippers, sandals, heels or sides open shoes.

  • 7. Do not wear contact lenses.

  • 8. No smoking, drinking and eating al all time in the laboratory.

  • 9. Do not throw waste organic liquids into the sink.

    • 10. Know the location of all safety equipment.

    • 11. Read the label on the container if a chemical properly.

    • 12. Use a hood for poisonous or irritating fumes.

    • 13. Throw all unused or contaminated chemical properly.

    • 14. Do not return used reagent to the stock bottle.

    • 15. Do not send your product with your report.

    • 16. Evacuate the laboratory when a fire alarm sounds.

    • 17. Turn off the flame and switch off the hot plate before leaving the laboratory.

    • 18. Always practice good housekeeping.

    • 19. Always add acids to water.

    • 20. Do not aim the opening of any glassware at yourself or anyone else.

    • 21. Do not use cracked or chipped glassware.

    • 22. Never use mouth suction when using a pipette.

    • 23. Report any accident in the laboratory.

    • 24. Do not leave any heating, vigorous or rapid reaction unattended.

    • 25. Do not make fun and joke in the laboratory.

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Experiment 1

BASIC LABORATORY TECHNIQUE

Objective:

  • 1. To use triple beam balance.

  • 2. To measure the weight using differentiating weighing method.

  • 3. To measure the accurate and inaccurate measuring liquid volume apparatus based on calculated volume from weight and density information.

  • 4. To record data using the right apparatus.

Concept:

  • 1. To know that each apparatus having its own accuracy.

  • 2. To record the correct data that corresponds to the accuracy of apparatus.

  • 3. To report the calculated result using data gain from measurement with the correct significant figures.

Introduction:

Laboratory experiment is an important part in chemistry course which required a good observation and utilization of right laboratory technique. Through the experiment, student will be exposed on basic and appropriate methods in Chemistry.

It is important to record the correct measuring number in order to show the accuracy of apparatus. This technique involved the concept of significant figures and round-up numbers.

Weighing: Triple Beam Balance and Electrical Balance

Triple beam balance was created to weigh with the accuracy near to 0.0 gram (one decimal point) and for electrical balance is near to 0.0000 gram. The basic principle for modern balance is to vary the weight of material which is unknown with the known weight.

Warning: Balance is easy to breakdown. Use carefully.

Weighing Volume

The volume measurement can be carried out using measuring cylinder, pipette, burette, volumetric flask etc. Volumes measurement made using pipette and burette are more accurate than measuring cylinder.

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Apparatus:

Triple beam balance Weighing bottle Erlenmeyer flask Burette Pipette Beaker Measuring cylinder

4 x 250 mL 1 x 50 mL 1 x 25 mL 1 x 50 mL or 25 mL 1 x 50 mL or 25 mL

Material:

Water

Coin

1 cent x 20

Method:

  • A. Weighing

Using triple beam balance and electrical balance, measure the weight of coins and record the data.

  • B. Volume measurement

    • 1. Ensure the apparatus is clean before use. Wash if necessary.

    • 2. Label Erlenmeyer flask as A, B, C and D, weigh and record the weight of each flask.

    • 3. By using burette, put 25 mL of water into flask A. Record the burette reading to the nearest 0.05 mL.

    • 4. Transfer 25 mL water into flask B by using pipette.

    • 5. Weigh and record the weight of each flask with water.

    • 6. Transfer 25 mL water into flask C by using beaker and weigh again.

    • 7. By using measuring cylinder, measure and transfer 25 mL water into flask D and weigh again.

    • 8. From the volume and weight obtained, identify the accuracy of each apparatus (burette, pipette, measurement cylinder and beaker). Calculate water density by using the data obtained.

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Objective:

Experiment 2

DILUTION

To determine the concentration of coloured solution such as FeCl 3 by using dilution and colour differentiating (colorimetric) techniques.

Concept:

  • 1. To understand molarity, normality and mole concept.

  • 2. To learn dilution technique.

  • 3. To learn the way to use M 1 V 2 = M 2 V 2 equation in dilute liquid calculation.

Introduction:

Concentration can be expressed in many different ways such as percentage volume and percentage weight etc. In laboratory, normally concentrations were expressed as molarity and normality.

Molarity is the mole of material in 1000 mL (1 liter or 1 dm 3 ) of solution, as shown as followed equation:

Mole

Molarity (M) =

Volume (1 liter /1 dm 3 )

M = n / V

Stock solution is the solution with known concentration. When the solution was diluted, only the concentrations will change while the mole number is remain the same. Based on this principle, the concentration of dilute solution can be determined by using followed equation:

Where

M 1

V 1

M 2

V2

M 1 V 1 = M 2 V 2

= concentration of concentrated solution (mol dm 3 ) = volume of concentrated solution (dm 3 ) = concentration of dilute solution = volume of dilute solution

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Apparatus:

Burette

1 x 50 mL

Pipette

l x 5 mL

Test tube

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Material:

  • 0.10 M FeCl 3 solution

  • 0.10 M KCNS solution

FeCl 3 solution (B)

Method:

  • 1. Based on given equation, calculate and prepare the following solution from standard solution of 0.10 M FeCl 3 by using pipette.

    • a. 10mL FeCl 3 solution (5.0 x 10 -2 M)

    • b. 10mL FeCl 3 solution (1.0 x 10 -2 M)

    • c. 10mL FeCl 3 solution (5.0 x 10 -3 M)

    • d. 10mL FeCl 3 solution (1.0 x 10 -3 M)

    • e. 10mL FeCl 3 solution (5.0 x 10 -4 M)

Record the volume of solution used.

  • 2. Transfer each 5 mL of prepared solution into test tube and add 2 drops of KCNS (potassium thiocyanate) to each test tube. Shake it until homogen and wait for any colour changes.

  • 3. Transfer 5 mL of B solution into another test tube and add 2 drops of KCNS solution. Shake it and compare colour of the solution with the series of solution that have prepared previously (2). Suggest the concentrations of B solution.

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Experiment 3

ACID AND BASE TITRATION

Objective:

To determine the concentration of sodium hydroxide solution through titration technique using hydrochloric acid and sulfuric acid.

Concept:

  • 1. To determine the concentrations of acid and base solution through titration with standard solution.

  • 2. To apply the correct technique in titration.

  • 3. To carry out acid base titration using phenolphthalein as indicator.

Introduction:

Acid base titration involves a neutralization reaction in which an acid is reacted with an equivalent amount of base. For the neutralization of hydrochloric acid with sodium hydroxide:

HCl + NaOH H 2 O + NaCl

Neutralization occurs when acid and base exists in comparable stoichiometry, for instance the amount of hydrochloric acid (mole) is equivalent with the amount of sodium hydroxide (mole). The end point of titration can be determined using indicator.

Apparatus:

Volumetric flask

250 mL

Filter funnel Beaker Burette Pipette

1 x 250 mL 1 x 50 mL 1 x 25 mL

Material

  • a) 100 mL 1.000 x 10 -2 M HCl solution

  • b) 100 mL 1.000 x 10 -2 M H 2 SO 4 solution

  • c) 10 mL C solution containing NaOH (with pipette)

  • d) Phenolphthalein solution

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Method:

  • 1. Put 10 mL of C solution in volumetric flask, dilutes with distilled water to the mark and mixing thoroughly. Transfer the solution to a clean beaker. Label solution as C. Rinse a flask with water twice.

  • 2. Clean burette and rinse with 5 mL HCI solution (1.000 x 10 -2 M) twice. Place 25 mL of HCI solution (1.000 x 10 -2 M) to burette using funnel.

  • 3. Clean pipette and rinse twice using C solution. Pipette 25 mL of C solution in three Erlenmeyer flask. Add 2 drops of phenolphthalein indicator.

  • 4. Record the initial volume reading to the nearest two decimal points. Titrate C solution with HCI from burette to a colourless solution end point. Record the final volume reading and calculate the used acid volume. Note: phenolphthalein colour will be change from magenta (base) to colourless (acid)

  • 5. Repeat the titration until the different volume of acid is in the range of 0.003 for three experiments.

  • 6. Calculate the concentrations of NaOH solution concentrations of C.

(that was in flask) and the

  • 7. Repeat steps 3 to 7 by replace HCI with H 2 SO 4 .

Note:

This experiment is acid-base reaction. It is crucial to know the reaction equation and the way to calculate solution concentrations. The correct burette reading is important in this experiment.

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Experiment 4

HYDRATED SALT FORMULA

Objective:

  • 1. To determine the volume of water content in hydrated salt.

  • 2. To determine the formula of hydrated salt.

Material/apparatus

Crucible or test tube with cover Retort stand Bunsen burner Thermometer Balance Hydrated salt: CuSO 4 .xH 2 O

Method

  • 1. Heat crucible for a while.

  • 2. Weigh crucible with cover.

  • 3. Add approximately 2 gram of hydrated salt, weigh and record the data.

  • 4. Heat salt gradually in crucible without cover for around 3-5 minutes.

  • 5. Observe any colour changes.

  • 6. Stop heating, cover the crucible and wait until cool down.

  • 7. Observe.

  • 8. Weigh.

  • 9. Grind the salt using glass rod and heat again.

    • 10. Cool the salt to room temperature.

    • 11. Weigh again. Continue heating until the weight constant. *Cool the sample in desiccator if needed.

    • 12. Record the salt temperature after final weight.

    • 13. Add few drops of water at room temperature, record the temperature.

    • 14. Observe.

Calculation

  • 1. Calculate the mole number of hydrated salt, results of unhydrated salt and weight of leave water from this reaction

  • 2. If the formula of hydrated salt is CuSO 4 .xH 2 O, verify x. Compare with the real molecular formula.

  • 3. List any error sources. Comment the x value.

  • 4. What is the name of process when water release from hydrated salt, endothermic or exothermic process?

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Objective:

Experiment 5

CHARLES LAW

To study the effect of temperature to gas volume

Introduction:

Charles Law involve the gas expands when heated while weight and pressure are constant. As the temperature increases, the particle energy will be increased as a result of the increasing of particle movement.

Volume

Temperature (in Kelvin, K )

=

constant

If V 1 and V 2 is the different volume for the same gas when the weight is constant at temperature T 1 and T 2 , so:

V

V

1 =

2

T 1

T 2

Apparatus:

Stop watch, Erlenmeyer flask equipped with rubber stopper, rubber tube with clip, beaker (500 mL), Bunsen burner, thermometer, tripod stand

Method:

  • 1. Set up apparatus as shown in the figure. Weigh empty Erlenmeyer flask that equipped with rubber stopper and clip.

  • 2. Place Erlenmeyer flask in a beaker that containing water.

  • 3. Boil water for 10 minutes with the tube open so the air in flask will have similar temperature with water boiling point (100°C).

  • 4. Fill the sink with water while the air in flask still hot.

  • 5. As the heating continue, clip the rubber tube and mark the clip position.

  • 6. Remove that flask from boil water and place the end of tube together with clip into sink that containing water. Leave the flask in air.

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  • 7. Open the clip and let the water flow into the flask. Ensure the air temperature in flask decrease to the water temperature.

  • 8. Clip the tube at the point mark and remove flask from sink.

  • 9. Measure the volume of apparatus setup (flask equipped with tube and clip). You may weigh the apparatus setup and use the water density to get the volume or by filling the apparatus with water and measure the volume of water by filling it in volumetric cylinder.

10. Plot the volume versus temperature graph and extrapolate the graph to zero volume.

Question:

  • 1. What is the temperature (in Celsius) obtained when the extrapolated graph cross at temperature-axis? Compare with the theory result.

  • 2. Using Charles Law and the amount of gas volume at 100°C from your experiment, determine the volume theory at the water temperature in sink.

  • 3. Illustrate a graph for volume theory of water in sink in the same graph paper. Where did graph cross the temperature axis? Explain your data.

Example of experiment data:

  • a. Weight of equipped flask

=

g

  • b. Weight of equipped flask + water

=

g

  • c. Weight of equipped flask + full water

=

g

Data:

  • i. Weight of water in full flask =

 

g

ii.

Weight of sucked water (b-a)

=

g

iii. Volume of sucked water (ii x water density) =

g

iv. Volume of air at 100°C

= Volume of full water in flask

= (i) x water density

=

mL

______

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  • v. Volume of air in room temperature

= (Volume of air at 100 o C) –

(Volume of sucked water)

= (iv) – (iii)

13 v. Volume of air in room temperature = (Volume of air at 100 C) –

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Experiment 6

DISSIMILARITY BETWEEN ELECTROVALENT AND COVALENT BOND

Objective:

To differentiate the properties between covalent compound (either pure covalent or ionic covalent) and electrovalent compound

Introduction:

Electrovalence compound exist from the arrangement of positive ion and negative ion. In solution, both positive and negative ion was separated due to the existence of water molecule. If this ion was reacted with another ion and produce more strong compound, the reaction might be more reactive. This effect can be seen from the vigorous formation of sediment and gas released.

For covalent compound, the reactions slowly occur due to the low attractive forces. This compound is hardly to dissolve or solidify in polar solvent. Covalent compound that exist as a gas will produce acid or base solution when dissolve in water such as HCl and

ammonia gas (NH 3 ). Water soluble covalent compound is ionic covalent which produces ions when it is dissolve in water.

Electrovalent compounds are able to conduct electricity either in solution or melted but not in solid form. The ion will attracted to different pole where positive ion will receive electron whereby negative ion will donate electron.

Apparatus:

Test tube, 150 mL beaker, stopper, tube, battery, wire and bulb.

Chemical:

NaCl solution, C 2 H 5 Br liquid, H 2 O 2 liquid, AgNO 3 solution, NaOH solution, phenolphthalein, HCl solution, Na 2 CO 3 solid, Zn/Cu/C electrode, NH 4 OH solution, ethanol and NaCl solid.

Method:

Precipitation

  • 1. Prepare 3 clean test tubes and label as A, B and C.

  • 2. Fill test tube A with 5 mL NaCl solution, B with 5 mL C 2 H 5 Br liquid, and C with 5 mL H 2 O 2 liquid.

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  • 4. Observe.

  • 5. Record the precipitation time.

Gas released

  • 1. Fill 5 mL of NaOH solution in test tube and add 2 drops of phenolphthalein.

  • 2. Fill 5 mL HCl solution in another test tube equipped with glass tube.

  • 3. Add small amount of Na 2 CO 3 in test tube containing HCl. Observe either reaction occur or not. The gas release can be determined by inserting the glass tube into test tube containing NaOH.

  • 4. Record any changes and explain.

Electric conductivity

Setup apparatus as shown below

At least 3 units of 1.5V battery
At least 3 units of 1.5V battery
15 4. Observe. 5. Record the precipitation time. Gas released 1. Fill 5 mL of NaOH
  • 1. Fill HCl solution in beaker (half).

  • 2. Put Zn/Cu electrode in the solution.

  • 3. Switch on the circuit when all connection is correct.

  • 4. Observed either the bulb blink or not, if blink, clear or not.

  • 5. Switch off the circuit; replace the HCl solution with NaCl solution, NaOH solution, H 2 O 2 liquid and NaCl solid in ethanol.

Question:

  • 1. Describe whether this solution can be electrically conducting or have electrolyte properties: H 2 S solution, melt AgCl, HCl solution and melt FeS.

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Experiment 7

MOLECULAR GEOMETRY

Objective:

  • 1. To determine the geometry of molecule.

  • 2. To build 3 dimension model for molecule

Introduction:

Lewis structure provides a structure of atom together with the electron valence. It can be used to get the actual geometry structure for certain molecule or ion. The valence shell electron pair repulsion model (VSEPR model) is important in order to determine the structure of actual geometry structure. This model is based on the idea that groups of electron repels each other and will allocate themselves as far away from each other as possible within a molecule. An electron domain is a region in space where electrons can be found.

According to VSEPR theory, the shape of molecule is determined by the tendency of electron domains to keep as far away from each other as possible. To predict the shape of molecule or ion, we need to know how many sets of electron pairs surround the central atom. The sets of electron pairs include the amount of lone pair electron and the amount of bonding electron for central atom.

The sets of electron pairs will arranged themselves to minimize the repulsive forces within the molecule. The actual geometry molecule is based on the position of terminal atom that binds to central atom. The lone pair electron will only influence the bond angle.

Method:

  • 1. By using ball with 1, 2, 3, 4, 5 and 6 sticks, build following geometry:

    • - Linear Planar

    • - Trigon

    • - Tetrahedron

    • - Bypyramid trigon

    • - Octahedron

  • 2. Determine the angle for each geometry.

  • 3. Sketch each of the geometry and define the angle.

  • Geometry molecule for HCl, BH 3 , and CO 2

    • 1. Build HCl molecule model by using ball with 1 stick.

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    • 3. Build BH 3 molecule model using ball with 1 stick as the end atom and ball with 3 stick as central atom.

    • 4. Determine the geometry and bond angle for each molecule.

    Geometry molecule for CH 4 , NH 3 and H 2 O

    • 1. Build CH 4 , NH 3 and H 2 O geometry model using ball with one stick as the terminal atom and ball with 4 stick as central atom. To show the electron valence in molecule, leave one or two stick at central atom without ball which one stick is correspond to a pair or electron valence.

    • 2. Determine the geometry for CH 4 , NH 3 and H 2 O molecules.

    • 3. Determine the real angle bonding for each molecule using TTPE whether it less or equal with the basic angle.

    Molecular geometry for PF 5 , AsCl 5 , ICl 3 , XeF 2 , SF 4

    • 1. Build AsCl 5 and PF 5 molecules model using ball with 5 stick as central atom and ball with one stick as terminal atom.

    • 2. Determine the actual angle of these molecules.

    • 3. By using the same ball, build ICl 3 , XeF 2 and SF 4 molecules model and leave the stick without ball to show the lone pair electron for central atom. You might get the variety of arrangement; identify the most stable geometry for each molecule. Determine their actual angle.

    Molecular geometry for SF 6 , XeF 6 and BrF 6

    • 1. Build the model for molecule above by using ball with two stick as terminal atom, and ball with 6 stick as central atom.

    • 2. Restructure the possible geometry for XeF 4 and BrF 5 molecules and determine the most stable geometry for that molecule together with the angle.

    Question:

    • 1. What is the most important factor in order to determine the ion or molecule geometry?

    • 2. How to get the number of lone pair electron and the number of bonding pair electron so that you can use TTPE?

    • 3. Why the geometry molecule for H 2 O is non-linear compared to CO 2 ?

    • 4. Give the correlations between the basic geometry and hybridization for central atom.

    © RI/HB/AM/RIM 2007