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Chemistry Lab Manual
Chemistry Lab Manual
Introduction to Chemistry
CHM-102
Instructor: Dr. Mohsin Raza
Department of Chemistry
COMSATS University Islamabad
List of Experiments
5. Acid-base titration.
8. Gravimetric analysis.
Theory- The change from solid to liquid state of a compound in heating is called melting and the
temperature at which a solid in its pure form melts is called the melting point. Every pure solid has
a characteristics melting point therefore determination of melting point helps in identification of
the compound. Presence of impurities lowers the melting point of the solid. Thus Melting point
also serves as a criterion of purity of a compound.
Procedure-
1. Take a fine capillary of length 5-6cm. seal its one end by inserting the end of the capillary tube
horizontally into the extreme edge of a small steady Bunsen flame for a few seconds, rotating the
capillary mean while.
2. Take a small quantity of the compound whose melting point is to be determined on a porous
plate and powder it with a spatula.
3. Introduce the powdered compound in the capillary tube by introducing the open end of the
capillary tube into the powdered compound and gently rotating it. Gently tap the capillary tube
against the porous plate so that the compound sinks
into the closed end. Repeat the procedure of introducing and tapping three to four times.
4. Moisten the bulb of thermometer with Conc. Sulphuric acid or liquid paraffin and attach
the capillary to the lower end of the thermometer.
5. Place the thermometer with the capillary tube in the melting point apparatus containing
at least two third of its volume liquid paraffin in such a way that the closed end of the capillary
remains below the surface of Liquid paraffin.
6. Now heat the beaker gently and note down the temperature from time to time and finally
note down the temperature at which the compound starts melting and completely melts.
7. Repeat the experiment with a new capillary tube and fresh quantity of the substance.
Observations-
Melting point
1 ................................0C
2 ................................0C
3 ...............................0C
Precaution-
2. The rate of heating should be controlled. It should be very slow near the melting point
so that the melting point can be recorded accurately.
Experiment 2
Recrystallization
Recrystallization, also known as fractional crystallization, is a procedure for purifying an impure
compound in a solvent. The method of purification is based on the principle that the solubility
of most solids increases with increased temperature. This means that as temperature
increases, the amount of solute that can be dissolved in a solvent increases.
Introduction
An impure compound is dissolved (the impurities must also be soluble in the solvent), to
prepare a highly concentrated solution at a high temperature. The solution is cooled.
Decreasing the temperature causes the solubility of the impurities in the solution and the
substance being purified to decrease. The impure substance then crystallizes before the
impurities- assuming that there was more impure substance than there were impurities. The
impure substance will crystallize in a purer form because the impurities won't crystallize yet,
Figure 1
Figure 2
References
1. Petrucci, Harwood, Herring, Madura. General Chemistry: Principles & Modern Applications,
Ninth Ed. Upper Saddle River,NJ: Pearson Education, Inc., 2007.
Experiment 3
Materials Needed:
▪ Litmus paper (both red and blue)
▪ Test tubes
▪ Different solutions of known pH (e.g., acidic, neutral, and basic solutions)
▪ Distilled water (for rinsing)
▪ Droppers or pipettes
▪ pH scale or pH chart for reference
Procedure:
1. Preparation:
Gather all the necessary materials and safety equipment, including lab goggles.
2. Labeling Test Tubes:
Take several clean test tubes and label them with the names or pH values of the solutions you will
test. For example, label one "HCl" for hydrochloric acid, one "Water" for distilled water, and one
"NaOH" for sodium hydroxide.
3. Testing Acidic Solutions:
Take a test tube labeled "HCl" and add a small amount of hydrochloric acid (or any acidic solution
you want to test) to it.
4. Testing Neutral Solutions:
Take another test tube labeled "Water" and add a small amount of distilled water to it. Distilled
water is considered neutral (pH 7).
5. Testing Basic Solutions:
Take a test tube labeled "NaOH" and add a small amount of sodium hydroxide solution (or any
basic solution you want to test) to it.
6. Testing the Unknown Solution:
If you have an unknown solution to test, use a separate test tube and add a small amount of the
unknown solution to it.
7. Using Litmus Paper:
Cut small strips of both red and blue litmus paper. Make sure to use a clean pair of scissors for
each type of litmus paper to prevent contamination.
Dip the red litmus paper strip into each test tube and observe the color change. Red litmus paper
turns blue in a basic solution but remains red in acidic or neutral solutions.
Dip the blue litmus paper strip into each test tube and observe the color change. Blue litmus
paper turns red in an acidic solution but remains blue in neutral or basic solutions.
8. Observation and Interpretation:
Record your observations for each litmus paper strip in each test tube.
Use a pH scale or pH chart for reference to determine the approximate pH value of each solution
based on the litmus paper color changes.
9. Concluding Remarks:
Based on your observations and the litmus paper color changes, identify and record the pH of
each solution.
If you tested an unknown solution, determine its pH based on the litmus paper results.
10. Cleanup:
Properly dispose of any waste solutions and used litmus paper.
Clean and rinse the test tubes and other equipment for future use.
Notes: Determination of pH using Litmus Paper
Introduction:
Theory:
▪ Litmus paper comes in two primary forms: red and blue.
▪ Red litmus paper is blue in a basic (alkaline) solution and remains red in an acidic or
neutral solution.
▪ Blue litmus paper is red in an acidic solution and remains blue in a neutral or basic
solution.
▪ The color change in litmus paper is due to the presence of specific pigment molecules
that undergo structural changes depending on the pH of the solution.
▪ Litmus paper provides a qualitative assessment of pH. It does not provide a precise pH
value but can indicate whether a solution is acidic, neutral, or basic.
▪ When litmus paper changes color, it helps classify the pH of a solution into one of three
categories:
▪ Acidic (pH < 7): Red litmus paper turns blue.
▪ Neutral (pH = 7): Litmus paper retains its original color.
▪ Basic (pH > 7): Blue litmus paper turns red.
Conclusion:
▪ Litmus paper is a useful qualitative indicator for assessing the pH of solutions.
▪ It can quickly determine whether a solution is acidic, neutral, or basic based on observed
color changes.
▪ For precise pH measurements, more accurate pH meters or indicators are used.
Experiment 4
Objective:
To calibrate and verify the accuracy of volumetric glassware by measuring the volume of a liquid
and comparing it with the calibrated volume.
Materials Needed:
Procedure:
1. Preparation:
Ensure that all glassware is clean and dry. Rinse the glassware with distilled water to
remove any contaminants. Allow it to dry thoroughly.
2. Determining the Mass of Water:
Weigh a clean, dry, empty beaker on the analytical balance. Record the mass as "m1."
3. Filling the Volumetric Glassware:
Choose one of the volumetric glassware items (e.g., a 100 mL volumetric flask).
Using a funnel, carefully add distilled water to the flask to approximately 80-90% of its
calibrated volume. This minimizes potential errors due to surface tension.
4. Measuring the Volume:
Read and record the exact level of the meniscus in the volumetric glassware. The bottom
of the meniscus should align precisely with the calibration mark. This is your initial volume
reading.
5. Weighing the Filled Glassware:
Carefully pour the water from the volumetric glassware into the pre-weighed beaker.
Weigh the beaker with the water on the analytical balance and record the mass as "m2."
6. Calculating the Volume:
Calculate the volume of water using the formula:
Volume (mL) = m2 - m1
(Note: 1 mL of water has a mass of approximately 1 g at room temperature.)
7. Comparing the Measured Volume with Calibration:
Compare the measured volume (step 6) with the calibrated volume of the glassware.
Determine the percentage error by using the formula:
Percentage Error = [(Calibrated Volume - Measured Volume) / Calibrated Volume] x 100
Repeat the above steps with different pieces of volumetric glassware (e.g., a pipette or
burette) to assess their calibration and accuracy.
Figure 3.1: Placement of the meniscus. The left view shows what it looks like from the side, while the
right view shows what it looks like isometrically.
Safety Precautions:
Acid-Base Titration
Objective:
To determine the concentration of an unknown acidic or basic solution by titrating it with a
standardized solution of known concentration.
Materials Needed:
3. Sample Preparation:
Measure a known volume (e.g., 25.00 mL) of the unknown solution using a pipette and
transfer it to the labeled conical flask.
4. Adding Indicator:
Add a few drops of a suitable pH indicator (e.g., phenolphthalein or methyl orange) to the
conical flask. The indicator will change color during the titration to signal the endpoint.
5. Titration:
Place the conical flask with the unknown solution on the bench.
Slowly add the standard solution from the burette to the conical flask while swirling the
solution gently. Continue adding the standard solution drop by drop as you approach the
endpoint. The solution in the conical flask will change color at the endpoint, indicating the
neutralization of the unknown solution.
6. Endpoint Detection:
The endpoint is reached when the indicator changes color, signaling that the reaction is
complete.
Materials Needed:
Procedure:
1. Preparation:
Label the conical flask "Tap Water Sample" and the burette "Silver Nitrate Solution."
Rinse the burette with distilled water and then with the silver nitrate solution to ensure it
is clean and free from contaminants.
3. Sample Preparation:
Measure a known volume of the tap water sample (e.g., 50.0 mL) and transfer it to the
labeled conical flask.
4. Adding Indicator:
Add a few drops of potassium chromate (K2CrO4) indicator solution to the conical flask. The
indicator will change color during the titration to signal the endpoint.
5. Titration:
Place the conical flask with the tap water sample on a lab bench or suitable platform.
Carefully add the standardized silver nitrate solution drop by drop from the burette while
gently stirring the solution. The silver nitrate solution will react with the chloride ions in
the tap water sample.
6. Endpoint Detection:
Continue to add the silver nitrate solution until the indicator solution changes color, from
yellow to red-orange. The change in color indicates that all chloride ions in the tap water
sample have reacted with the silver ions.
Here's how you can calculate the chloride concentration in the tap water sample:
2. Environmental Impact:
High chloride levels in water can be harmful to aquatic ecosystems, especially in freshwater
bodies. Conducting this experiment helps in evaluating and mitigating the environmental
impact of chloride pollution from various sources like road salts and industrial discharge.
3. Health Concerns:
Chloride levels in drinking water are regulated due to potential health concerns. High chloride
concentrations may indicate the presence of other contaminants, such as heavy metals, which
can have adverse health effects if consumed in large quantities.
4. Corrosion Control:
The chloride concentration in water is directly related to its corrosivity. High chloride levels
can accelerate the corrosion of metal pipes, plumbing, and appliances. By monitoring chloride
levels, water utilities can take preventive measures to reduce corrosion and extend the
lifespan of infrastructure.
The objective of this experiment is to prepare a buffer solution using acetic acid and sodium acetate,
applying the Henderson-Hasselbalch equation, and verifying its pH control to enhance understanding of
buffer systems in practical applications.
1. Weak acid and its conjugate base or weak base and its conjugate acid.
2. Distilled water.
3. pH meter or pH indicator paper.
4. Graduated cylinders or volumetric flasks.
5. Stirring rod or magnetic stirrer.
6. Beakers or containers for mixing.
Steps:
Select a weak acid and its conjugate base, or a weak base and its conjugate acid, based on the desired
pH of the buffer. Common examples include acetic acid (CH₃COOH) and acetate ion (CH₃COO⁻), or
ammonium ion (NH₄⁺) and ammonia (NH₃).
Determine the molar ratio of the weak acid to its conjugate base (or weak base to its conjugate acid)
that will give the desired pH. This ratio is often expressed as the Henderson-Hasselbalch equation:
[𝐴− ]
𝑝𝐻 = 𝑝𝐾𝑎 + log( )
[𝐻𝐴]
Where [A−]is the concentration of the conjugate base, [HA] is the concentration of the weak acid,
and pKa is the negative logarithm (base 10) of the acid dissociation constant (Ka).
3. Measure Components:
Measure the appropriate volumes of the weak acid and its conjugate base (or weak base and its
conjugate acid) using graduated cylinders or volumetric flasks.
5. Check pH:
Use a pH meter or pH indicator paper to check the pH of the resulting solution. Adjust if necessary by
adding more acid or base.
If the concentration of the buffer needs adjustment, dilute the solution with distilled water.
7. Final Mixing:
Notes:
• The concentrations of the weak acid and its conjugate base (or weak base and its conjugate acid)
depend on the desired buffer capacity and the specific application.
• Always use high-quality reagents and precise measurements for accurate results.
• It's crucial to know the pKa of the weak acid in the selected pair to calculate the ratio accurately.
Calculation Steps:
[𝐴− ]
log([𝐻𝐴]) = - 0.06
[𝐴− ]
[𝐻𝐴]
= 10-0.06
[𝐴− ]
≈ 0.798
[𝐻𝐴]
2. Calculate Concentrations:
Choose a convenient total concentration (e.g., 0.1 M). This means [A−] ≈ 0.798 × 0.1 and [HA] ≈
0.1
3. Measure Components:
Measure 0.1 M acetic acid and 0.0798 M sodium acetate using graduated cylinders or volumetric
flasks.
5. Check pH:
Use a pH meter or pH indicator paper to check the pH of the resulting solution. Adjust, if
necessary, by adding more acetic acid or sodium acetate.
If the concentration of the buffer needs adjustment, dilute the solution with distilled water.
7. Final Mixing:
Objective:
To determine the amount of barium in a given sample of barium chloride through gravimetric
analysis.
Materials:
Procedure:
Preparation of the Sample:
Weigh 2.0 grams of barium chloride using an analytical balance.
Transfer the weighed sample into a beaker.
Dissolution of Barium Chloride:
Add 50 mL of distilled water to the beaker containing the barium chloride.
Stir the solution until the barium chloride completely dissolves.
Precipitation of Barium Sulfate:
Add 10-15 drops of hydrochloric acid (HCl) to the solution. This is to prevent the precipitation of
other metal ions as hydroxides.
Slowly add 20 mL of a dilute solution of sulfuric acid (H₂SO₄) to the solution with constant stirring.
This causes the precipitation of barium sulfate (BaSO₄) according to the reaction:
Filtering and Washing:
Allow the barium sulfate precipitate to settle.
Filter the precipitate using filter paper and a funnel.
Wash the precipitate thoroughly with distilled water to remove any soluble impurities.
Drying the Precipitate:
Transfer the wet precipitate to a crucible.
Dry the precipitate by gently heating it over a Bunsen burner until a constant weight is achieved.
Weighing the Barium Sulfate:
Weigh the crucible containing the barium sulfate precipitate using an analytical balance.
Record the mass.
Calculations:
Calculate the mass of barium sulfate formed. Since the molar ratio of barium to barium sulfate is
1:1, this mass is equal to the mass of barium in the original sample.
Calculate the percentage of barium in the sample.
Percentage of Barium = (Mass of Barium in Barium Sulfate / Initial Mass of Barium Chloride) × 100
Safety Precautions:
• Handle hydrochloric acid and sulfuric acid with care. Wear appropriate protective gear,
including gloves and goggles.
• Work in a well-ventilated area.
• Use crucible tongs when handling hot crucibles.
• Follow standard laboratory safety procedures.
The chemical reactions involved in the gravimetric analysis of barium chloride involve the
precipitation of barium sulfate (BaSO4)
4. Overall reaction:
The overall reaction for the precipitation of barium sulfate from barium chloride can be
represented as follows:
It's important to note that in the actual experimental procedure, hydrochloric acid is added before
sulfuric acid to prevent the precipitation of other metal ions as hydroxides. The sequence of the
addition of reagents is designed to ensure the selective formation of the barium sulfate
precipitate.