Introduction

Laboratory reporting format

Generally, lab reports should include the following elements.
I. Cover page
The cover page contains title of the experiment, experiment no, group name, section, date you
made the experiment as well as the date you hand in the report (Date of Practical and Hand in
Date)
II. Body part
1.
Experiment number 5. Apparatus and 8. Result and discussion
2. Title chemicals 9. Conclusion
3. Objective 6. Procedure
4. Theory 7. Observation and data
Laboratory safety rules and regulations
Safety is a prime requisite for laboratory work. At all times when you are working in the
chemistry laboratory you should do the following.
 Wear safety goggles all the time in the laboratory.
 Lab coats should be worn when working in laboratory
 Accidents: first aid is essential .
 Learn the location of the safety equipment: fire extinguisher, safety shower, and
eye wash fountain.
 Injuries/accidents should be immediately reported to your instructor.
 No use of any food or drink in laboratory
 Keep your bench area and reagent table clean and tidy at all times.
 Long hair is to be constrained. Like hanging clothes, long hair is subject to fire and
contact with chemicals. A rubber band will be used to constrain particularly long hair if
necessary.
 WASH YOUR HANDS! Wash your hands frequently during lab, and definitely wash
your hands twice at the end of the lab
 Do NOT apply makeup (including Chapstick and other lip balms) in the lab.

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  Should an injury occur, regardless of how minor it is, report it IMMEDIATELY to the
lab supervisor.
 Never pick up broken glassware with your bare hands,
 NEVER put broken glass in a regular garbage can. A container is provided that is
especially designed for broken glassware.
 Always read the labels to reagents (chemicals used in an experiment) twice!
 Never use reagents from an unmarked bottle.
 If you are not feeling well, report it to the laboratory supervisor immediately.
 Avoid bringing excess coats, books, backpacks or other personal items to the laboratory.
 Never smell a chemical straight out of a container.
 NEVER use a fire extinguisher on a person.
 If a fire should occur in a beaker or some other container, cover it with a glass dish or
other flame-retardant item.
 NEVER move ANY object that is burning.

Experiment-1
Mass and Volume Measurement
Accuracy: It is the deviation from the true value, (is a measure of systematic error). It is often
estimated as the deviation of the mean from the true value: accuracy = mean - true value. The
true value may not be known. For the purpose of comparison, measurement by an established
method or by an accredited institution is accepted as the true value. Precision: is a measure of
reproducibility and is affected by random error. Since all measurements contain random error,
the result from a single measurement cannot be accepted as the true value. An estimate of this
error is necessary to predict within what range the true value may lie, and this is done by
repeating a measurement several times. Precision can be explained interims of standard
deviation, relative standard deviation and coefficient of variance. Sensitivity: The sensitivity of a
method (or an instrument) is a measure of its ability to measure small amount or concentrations.

Measurement of mass

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Laboratory balances of several types and models, having varying degree of sensitivity, are
available for chemistry laboratory. The triple beam and the top-loading are the most common.
Some of them are given in the table below.

Balance Sensitivity (g)

Triple beam balance + 0.01
Top-loadng (having different + 0.01 - 0.0001
model)
Analytical (Electronic) balance + 0.00001

Analytical balances are used to weigh very small samples very accurately, while top-loading
balances are used when accuracy is not as important. The triple-beam balance is one type of
manual balance.

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Fig. 1 Types of balances

Procedure:
1. Check that the pan is empty and it is at zero point
2. Level the balance by screwing its movable feet until it points at the 0 scale.
3. Take the object to be weighed and place on the pan.
4. Manipulate the beam until the weight is balanced.
5. Record the mass of the object.
6. Repeat the procedures several times.

Note: Report your result as mass + D, where D is the deviation from the accepted value
Question:

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Calculate: Error, %Error SD, RSD and CV
Compare the balances interims of sensitivity, accuracy and precision.
Volume Measurement
Objective:
To attain skills in the use of volumetric glass wares.
Theory:
The fundamental unit of volume is the liter (L), defined as the volume occupied by 1Kg of water
at the temperature of maximum density (40C) and at 1 atmospheric pressure.
Various of types of equipment are used in the lab to measure volume. Beakers are used for
rough volume measurements of large amounts of liquid while graduated cylinders are used for
more precise measurements. Burettes and pipettes are used for very precise measurement.
The choice of a suitable device for measuring volume will depend on both the amount of liquid
you want to measure, and the level of accuracy needed. In general, you should use the smallest
measuring device available that is large enough to hold the volume of liquid you wish to
measure. Using a measuring device several times (because it is too small to measure the full
amount required). Conversely, using a measuring device that is too big also reduces accuracy.

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When measuring volume of a liquid, always read from the bottom of the meniscus, as shown
below. Position the eye horizontally at the bottom of the meniscus to read the level of the liquid.
The meniscus is a curve in the surface of the liquid caused by surface tension and by the
attraction between the liquid and the sides of the container.

Fig.2 Reading the meniscus

Procedure:
1. Using Burette

 Always use a small funnel to fill a burette.

 Always rinse a burette before use by rinsing the burette and burette tap (stopcock) with
the liquid that is going to be used before use. This will remove possible contaminants or
diluents.

 Fill the burette, slowly towards the end, and allow funnel to drain empty before adding
more, to prevent overflowing.

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  Leave an air gap between the funnel and the burette to allow air to escape as the burette is
being filled.

This will prevent air being forced out through the funnel resulting in spillage of the
funnel's contents.

 Fill the burette past the zero mark and drain until reading zero or below zero noting the
reading.

 The burette level is read from the bottom of the liquids curvature (meniscus)

 You can read most 25 ml and 50 ml burettes to 0.05 ml resolution by reading in between
the 0.1 ml markings.

2. Filling the pipette

 Squeeze out the air in the pipette helper bulb. Newer pipette helpers have a large lever
that is pushed to squeeze the suction bulb inside the apparatus.
 Position one hand on the pipette helper with the thumb on the fill/empty lever.
 Use the other hand to hold the lower container (beaker) and to stabilize the lower end of
the pipette.
 Position the pipette’s tip a little bit off the bottom of the container.
 Push the Fill/Empty lever up to fill the pipette
 Control the speed of the filling operation by adjusting how far you push the Fill/Empty
lever
 Stop filling when the meniscus is resting on top of the Fill Line. It may be necessary to
fill and/or empty the pipette by pressing the Fill/Empty lever up or down to properly
position the meniscus.

Note: Always keep the tip of the pipette immersed in liquid when filling to avoid drawing air
into the pipette helper. Never point a filled pipette upward or lay a filled pipette down on
the bench-top as liquid may reach the pipette helper and plug it . Never draw liquid into the
pipette helper. If you do, please alert the instructor immediately.

Emptying the pipette

· Position the filled pipette over the appropriate container
· Press the Fill/Empty lever downwards until the pipette is empty

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· Touch the tip of the pipette to the wall of the container to remove the drop that
may be clinging to the tip
· A small amount of liquid will remain in the tip of the pipette.
When finished with your pipette, be sure to place it in the dirty pipette holder/basket
pointing upward. This will keep the fragile tip from being damaged.
Questions:
1. Compare the precision of each measuring devices.
2. What do you do; if the last bit of liquid is remains in the pipette after the delivery?
3. Which finger should be used to control the volume of the liquid in the pipette?

Experiment-2
Physical and Chemical Change
Objectives:
 To make observations in before and after a change has been induced.
 Interpret the results of a test to determine if a compositional change has occurred.
Theory:
Chemical change is any change that results in the formation of new chemical substances. At the
molecular level, chemical change involves making or breaking of bonds between atoms. There
may be clues that a chemical reaction took place, such as light, heat, color change, gas
production, odor, or sound.

These changes are chemical:

 iron rusting (iron oxide forms)

 gasoline burning (water vapor and carbon dioxide form)
 eggs cooking (fluid protein molecules uncoil and crosslink to form a network)
 bread rising (yeast converts carbohydrates into carbon dioxide gas)
 milk souring (sour-tasting lactic acid is produced)
 suntanning (vitamin D and melanin is produced)

Physical change- rearranges molecules but doesn't affect their internal structures.

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Physical changes are concerned with energy and states of matter. A physical change does not
produce a new substance. Changes in state or phase (melting, freezing, vaporization,
condensation, sublimation) are physical changes. The starting and ending materials of a physical
change are the same, even though they may look different.

Some examples of physical change are:

 whipping egg whites (air is forced into the fluid, but no new substance is produced)
 magnetizing a compass needle (there is realignment of groups ("domains") of iron atoms,
but no real change within the iron atoms themselves).
 boiling water (water molecules are forced away from each other when the liquid changes
to vapor, but the molecules are still H2O.)
 dissolving sugar in water (sugar molecules are dispersed within the water, but the
individual sugar molecules are unchanged.)

Apparatus:

Test tube, Rubber stopper, Evaporating dish, Watch glass, Wire gauze, Bunsen burner.

Chemicals:

NaCl, NaNO3, NH3, Cu and Fe metals, Hydrated CuCl2

Procedure A:

1. Add a scoop of sodium chloride to a medium test tube. Fill the tube about half way with
distilled water. Put a solid rubber stopper to fit and shake to see if you can dissolve the
salt. Record what happened throughout this part.
Procedure B:

2. Pour half of your sodium chloride solution into an evaporating dish and leave half in the
test tube. Use the evaporating dish in part C.
3. Add several drops of silver nitrate solution (AgNO 3) to the test tube. Mix by swirling the
tube using the Cornell method. Record what you see in the tube. Be sure to notice any
differences from earlier materials.

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Procedure C:

4. Add several drops of the six molar ammonia: 6M NH 3 into the tube from part B. Quickly
put the cap back on the ammonia as well as the solid stopper on the tube. Gently swirl the
tube to mix the solutions. Record your observations.
5. Rinse the tube and contents down the drain with plenty of water.
Procedure D:

6. Place the evaporating dish with the sodium chloride solution that you made in part B,
onto a wire gauze placed upon an iron ring. Be sure the iron ring is first secured to the
ring stand a few centimeters above the top of a laboratory burner. Place a watch glass
over the evaporating dish (use the watch glass like a bowl, not like a dome).
7. Heat the solution until boiling then turn down the heat and simmer until all the moisture
is gone, including any drops on the underside of the watch glass.
8. Turn off the burner and LET THE APPARATUS COOL FOR AT LEAST 15
MINUTES. You may go on to another part of the lab and come back to finish after it has
cooled.
9. After it is only slightly warm when you place the back of your hand close to the dish,
examine the material inside the evaporating dish. You should notice that it is very similar
to the original sodium chloride. Record all observations.
10. Clean the dish and watch glass down the sink.
Procedure E:

11. Fold up a copper wire and place it inside a small test tube. Cover the wire with silver
nitrate solution. Set the tube aside for 10-15 minutes. Return later and record all
observations.
12. carefully dump the contents of the tube into the trash, rinsing with a water bottle.
Procedure F:

13. Place a small scoop of cobalt chloride hydrate into an evaporating dish. Heat it slowly
until it dries and changes color.
14. Turn off the burner and LET THE DISH COOL FOR AT LEAST 15 MINUTES. After
it has cooled add some water to the dried solid. Record all observations from this part.
Questions

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Identify the following processes as physical or chemical change.
1. Sugar dissolves in warm water
2. A nail rusts.
3. A glass breaks.
4. A piece of paper burns.
5. Iron and sulfur mix and form a partially magnetic black and yellow mixture.
6. Iron and sulfur are heated and form a non-magnetic shiny grey substance.
7. Dry Ice (solid carbon dioxide -- CO2) is sublimed at room temperature.
8. Vinegar reacts when mixed with baking soda.
9. Water boils at 100 degrees Celsius
10. Zinc when immersed in Hydrocholoric Acid produces hydrogen gas.

Experiment-3
Preparation of solutions
Objectives:

 To prepare solutions from solids and liquids

Theory:
Solution is a homogeneous mixture created by dissolving one or more solute in a solvent. The
solution with accurately known concentration is called standard (stock) solution. Solution can be
defined as a homogeneous mixture of two or more substances having uniform properties
throughout.

Solution is a mixture consisting of a solute and a solvent.

 Solute is component of a solution present in the lesser amount.

 Solvent is component of a solution present in the greater amount.

A stock solution is prepared by weighing out an appropriate portion of a pure solid or by

measuring out an appropriate volume of a pure liquid and diluting to a known volume.

3.1 Preparation of solution from soluble solids

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To prepare a solution that contain specified concentration of substance, it is necessary to dissolve
desired number of mole of solute in enough solvent to give desired final volume of solution.
Molarity is the most commonly used unit of concentration in chemistry, and defined as the
number of mole of solute per one liter of solution.

General procedure,
1. Weigh out the solid solute to the required molar solution
2. Carefully transfer the solid to volumetric flask that contains some amount of solvent large
enough to dissolve to solid.
3. Dissolve the sold swirling
4. Add solvent until the solution reaches the mark of volumetric flask.

3.2 Preparation of solutions from liquids

Commercially available acids and bases are labeled with concentration unit w/w % and specific
gravity (sp.gr) but not with molarities. These concentration units can be converted into molar
concentrations and then less concentrated solutions can be prepared by dilution.

The concentration unit w/w % can also be converted into normality using the following equation.

3.3 Diluting solution of known concentration

Dilution is the process of adding more solvent to produce solution of less concentration. Usually
diluted solution is prepared from small volume of more concentrated stock solution. The moles
of solute present in volume of delivered stock solution are equal to the moles present in diluted
solution.

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 Moles of solute before dilution = Moles of solute after dilution
The mole of solute is defined as the molarity of solution (M) of solution times the volume (V) of
the solution.
M1V1=M2V2
Where, M1-Molarity before dilution V1- volume before dilution M2- Molarity after dilution V2-
volume after dilution
Preparation of solutions with worked examples

Preparing a solution of known concentration is perhaps the most common activity in any
analytical laboratory. There are two methods for preparing solutions. These are:

1. Preparation of stock solutions

A stock solution is prepared by “weighing out an appropriate portion of pure solid” or by

“measuring out an appropriate volume of a pure liquid and diluting to a known volume”.
Exactly how this is done depends on the required concentration units. For example to prepare a
solution with desired molarity you would weigh out an appropriate mass of the reagent, dissolve
it in portion of solvent, and bring to the desired volume. To prepare solution where the solute
concentration is given as volume percent, you would measure out an appropriate volume of
solute and add sufficient solvent to obtain the desired total volume.

Example: Describe how you would prepare the following solutions: (a) 500 mL of
approximately 0.20 M NaOH using solid NaOH;

Solution: (a) Since the concentration only needs to be known to two significant figures, the mass
of NaOH and volume of solution do not need to be measured exactly. The desired mass of NaOH
is

0 .20 mol 40 . 0 g
× ×0 . 5 L
L mol = 4.0g

To prepare the solution we place 4.0 g of NaOH, weighed to the nearest tenth of a gram, in a
bottle or beaker and add approximately 500 mL of water.

2. Preparing Solutions by Dilution

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Solutions with small concentrations are often prepared by diluting a more concentrated stock
solution. A known volume of the stock solution is transferred to a new container and brought to a
new volume. Since the total amount of solute is the same before and after dilution, we know that
C o  V o = Cd  V d
where Co is the concentration of the stock solution, Vo is the volume of the stock solution being
diluted, Cd is the concentration of the dilute solution, and Vd is the volume of the dilute solution.
Again, the type of glassware used to measure Vo and Vd depends on how exact the solution's
concentration must be known.

Example: A laboratory procedure calls for 250 mL of an approximately 0.10 M solution of NH 3.

Describe how you would prepare this solution using a stock solution of concentrated NH 3 (14.8
M).

Substituting known volumes in equation, Co  Vo = Cd  Vd

14.8 M Vo = 0.10 M  0.25 L

and solving for Vo gives 1.69 x 10-3 L, or 1.7 mL. Since we are trying to make a solution that is
approximately 0.10 M NH3, we can measure the appropriate amount of concentrated NH3 using
a graduated cylinder, transfer the NH3 to a beaker, and add sufficient water to bring the total
solution volume to approximately 250 mL.

Experimental part

Apparatus: Electronic balance, beaker, volumetric flsks, graduated cylinders

Chemicals: NaCl, HCl, NaOH, and distilled water

Procedures
I. Preparation of solution from solids
a) Weigh 14.625 g of table salt (NaCl) on mass balance and dissolve in some amount of
distilled water not less than 5 mL in 250 mL volumetric flask. If it doesn’t dissolve yet
add some more water. If you are sure that the solid is completely dissolved add water to
the mark of volumetric flask. Label the prepared solution with sticker ‘1M’.

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 b) Weigh 5.8500g of NaCl on mass balance and dissolve completely in 100 mL volumetric
flask contain some water. After the solid completely dissolved fill up water to the mark of
volumetric flask. The prepared solution must labeled with sticker ‘0.1M’ .
c) Dissolve 4.000g of NaOH (caustic soda) pelates in 100 mL of water to get 100mL of 1M
solution.
Caution: when you weigh NaOH care must be taken to remove skin contact since it
attacks your skin.
II. Preparation of small concentrated solutions by dilution
a) Prepare 100mL of 0.5M and 100 mL 0.1 M NaCl solutions from (a) and
b) Prepare 50ml of 0.05 and 50 mL of 0.01M from (b).

III. Preparation of solution from more concentrated solutions (includes converting from
w/w % to most commonly used concentration units followed by diluting)
1. Prepare 250 mL of 0.1 M HCl aqueous solution. The concentrated HCl has specific
gravity of 1.18 g/mL and 37.2 % w/w of HCl.
2. Prepare 250 mL of 1M HNO3 (aq) from the stock solution(sp.gr = 1.42 g/mL and 70.5%
w/w). Caution avoid skin contact of even dilute HNO3 it reacts with skin protein and
turns you skin to yellow (xanthoprotein) at the point of contact.

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