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Self-Directed Learning (SDL)

Grade 11 Chemistry University Preparation (SCH3U)


Laboratory Manual.

Azza Kayal 582436

Instructor: Matt Roy

Due: March 8, 2015

Faculty of Education
Lakehead University

Note: In placement 1, I was assigned to teach grade 11 Chemistry University preparation. Thus,
due to time restriction I was not able to let the student perform the titration lab. Knowing that
titration is a crucial experimental procedure in chemistry, I have decided to have Titration
Analysis of Vinegar as part of my SDL activity.

Titration Analysis of Vinegar


1

Introduction:
Chemists often need to know the concentration of an acidic or basic solution. To acquire
this information, they use an experimental procedure called titration. In a titration, the
concentration of one solution is determined by quantitatively observing its reaction with a
solution of known concentration. The solution of known concentration is called a standard
solution. The aim of titration is to find the point at which the number of moles of the standard
solution is stoichiometrically equal to the original number of moles of the unknown solution.
This point is referred to as the equivalence point. At the equivalence point, all the moles of
hydrogen ions (H+) that were present in the original volume of one solution have reacted with an
equal number of moles of hydroxide (OH) ions from the other solution.
Precise volume measurements are needed when you perform a titration. Chemists use
special glass apparatus known as burette, Erlenmeyer flask and pipette to collect these
measurements (See Figure 1). As well, an acid base indicator is needed to monitor changes in
pH during the titration (see Figure 2).
In a titration, a pipette is used to measure a precise volume of standard solution into a
flask. The flask sits under a burette that contains the solution of unknown concentration. After
adding a few drops of indicator, you take an initial burette reading. Then you start adding the
known solution, slowly, to the flask (See Figure 3). The end point of the titration occurs when the
indicator changes colour. The indicator is chosen so that it matches its equivalence point.
2

Some definitions:
An Erlenmeyer flask (or conical flask) is the reaction vessel used in a titration. The most
common Erlenmeyer flask has a 250mL capacity.
A pipette is used to transferring precise and very accurate volumes of solution from a
storage container into an Erlenmeyer flask. By placing a squeezed rubber bulb over the wider
end, you can draw up the solution until the bottom of the meniscus (the curved water surface) is
level with the mark on the stem of the pipette. If you allow the solution to run into the
Erlenmeyer flask, leaving the small volume in the tip of the pipette, then the precise volume has
been transferred (See Figure 4).
A burette is a device for dispensing very precise volumes of solutions. When the first
solution has been placed in the Erlenmeyer flask using a pipette, the other reagent is added from
the burette, adjusting the rate of flow with the stopcock. It is vital to read the burette before you
start running in the second reagent since the volume added will be the difference between the
final and initial burette readings (See Figure 5 and 6).

1 Chemistry 11 (2001, Addison Wesley) page 399.


2 Chemistry 11 (2002, McGraw Hill Raerson) page 301.

Titration requirements:
For titration, a chemical reaction must be:
- Spontaneous chemicals react on their own without a continuous addition of energy.
- Fast chemicals react instantaneously when mixed.
- Quantitative the reaction is more than 99% complete
- Stoichiometric there is single, whole number mole ratio of amounts of reactants and
products.
In this investigation, you will be the quality control chemist. You have received a report that
a local high school cafeteria has been serving watered-down vinegar to the students. Your
purpose is to test the acetic acid concentration of the vinegar to discover whether it has been
diluted (i.e., below the 5.0% W/V acetic acid indicated on the purchased container).
Question:
What is the molar concentration of acetic acid in a sample of vinegar?
Prediction:
The manufacturer claims on the label that the vinegar container contains 5.0% acetic acid, which
translates into 0.87 mol/L concentration of acetic acid. The concentration of acetic acid in the
vinegar sample should be the same.
Experimental Design:
A sample of vinegar from the school cafeteria is diluted by a factor of 10 to make a 100mL
solution. The diluted solution is titrated with a standard sodium hydroxide solution using
phenolphthalein as the indicator.
Materials:
Lab apron
Two 250mL Erlenmeyer flask
Eye protection
NaOH (aq)
Vinegar
Phenolphthalein
Wash bottle of distilled water
Two 150mL beakers
250 mL beaker
100 mL volumetric flask with stopper
50mL burette
10mL volumetric pipette
Pipet bulb
Ring stand
Burette clamp
Stirring rod
Small funnel

3 Chemistry 11 (2002, Nelson) page 395

Preparing the NaOH(aq) solution


Prepare 2L of approximately 0.1 mol/L NaOH for standardization. Use 50% NaOH (w/w)
(Density = 1.53 gm/ml) solution which has been filtered or allowed to settle (do not shake or
agitate this solution). (You must calculate the amount of this solution needed.) Use distilled water
to prepare the NaOH solution. The solution should be stored in a polyethylene bottle since
sodium hydroxide dissolves silica from glass. The slow diffusion of CO2 through the plastic will
not be a problem during the duration of the experiment. Minimize the exposure of this solution to
air. Mix the solution thoroughly before using. The solution may settle between labs, so always
mix thoroughly before use.
How do we know the exact concentration of NaOH?
The solution is simple enough, we standardize the NaOH solution by using it to titrate a solution
of Potassium Hydrogen Phthalate (KHC8H4O4), which is frequently abbreviated KHP. Here the
KHP is acting as a primary standard. Primary Standards are extremely stable solids that can be
weighed out very accurately and used to standardize titrant solutions whose concentration is not
accurately known.
By knowing the mass of the KHP, we can determine the number of moles NaOH used in the
titration and thus determine its concentration.
Procedure:
Standardization of NaOH
1. Weigh out ~0.715g of KHP on the filter papers provided.
2. Transfer this to a 250 mL Erlenmeyer flask. Wash any residual KHP off the filter paper
into the flask. Dissolve in 50 mL distilled water.
3. Add a 2 to 3 drops Phenolphthalein.
4. Titrate to the endpoint with your NaOH solution. For the 50mL burettes used in this
titration, all volume readings can be made with a precision of 0.02 mL. Check with your
instructor to make sure you are reading the burette with sufficient precision.
5. Repeat this process for a total of three trials. Check with your instructor to make sure the
results are sufficiently close to each other (with a total difference of 0.1mL). If the
results are not sufficiently close together, repeat the titration a fourth time.
Titration of vinegar
1. Obtain about 30 mL of vinegar in a clean, dry 100 mL beaker.
2. Pipet one 10.00 mL portion into a clean 100mL volumetric flask and dilute to the
mark
3. Stopper and invert several times to mix thoroughly
4. Set up the 50 mL burette with NaOH(aq), following the accepted procedure for rinsing
and cleaning the burette.
5. Pipet a 10.00 mL sample of diluted vinegar into a clean Erlenmeyer flask.
6. Add 2 to 3 drops of phenolphthalein indicator.
7. Record the initial burette reading to the nearest 0.1 mL
8. Titrate the sample with NaOH(aq) until a single drop procedures a permanent change
from colourless to faint pink.

9. Record the final burette reading to the nearest 0.1 mL.


10. Repeat steps 6 to 10 until three consistent results are obtained.
When done properly a single drop of base will cause a permanent colour change signifying the end point of the titration
Note: If you overshoot the endpoint of the titration (a dark pink) you must repeat the trial.
When finished
a)
discard any leftover solutions in the sink once you have ensured that your
neighbours do not require it
b)
rinse the beakers and Erlenmeyer flasks well with tap water and put the glassware
away
c)
rinse the burette with distilled water, then with 5mL HCl (aq), then 3 more times
with distilled water
d)
Place the burette in the burette container.

Figure 1: The apparatus needed to perform a titration.

Figure 2: Acid/Base indicators with pKa values and colour change.

NaO
H

Vinegar +
pnptl*

Figure 3: Proper titration set up. (*Phenolphthalein)

Figure 4: The proper way to piette and transfer the solution to the Erlenmeyer flask.

Figure 5: The proper way to read the volume in a burette

Figure 6: The proper way to handle/load a burette.


Observations:
Table1: determining the concentration of NaOH (aq)
Mass (g)
Trial #1
Trial #2
Empty container
Container + KHP
KHP mass
Initial burette
reading (NaOH) mL
Final burette
reading (NaOH) mL
Volume of NaOH
used (mL)

Trial #3

Table2: determining the concentration of acetic acid


Trial #1

Trial #2

Trial #3

NaOH (aq)

NaOH (aq)

NaOH (aq)

Initial Volume
Reading (mL)
Final Volume
Reading (mL)
Total Volume
(mL)

Analysis
1.
2.

3.
4.
5.
6.
7.
8.

Write a balanced molecular equation for the reaction occurring between acetic acid and
sodium hydroxide. (4 marks)
Make a single set of calculations for the following calculations for trial #1 only: (3
marks)
a)
the volume of acetic acid used
b)
the volume of NaOH(aq) used
c)
the number of moles of acetic acid used
What type of reaction is occurring in the lab? (1 mark)
Based on your answers to questions 2c and 3, what is the number of moles of NaOH(aq)
required for titration be for Trial #1? (3 marks)
What is the concentration of the unknown acetic acid solution based on your info from
Trial #1? (2 marks)
Calculate the average concentration of acetic acid from the 3 trials. Show all of your
work for calculating this average. (3 marks)
List 3 acceptable sources of error for this lab. Discuss how each might affect the
calculated value of acetic acid. (3 marks)
Write a brief concluding statement.

Evaluation:
(a) Evaluate your evidence: how confident are you that your techniques and measurements
resulted in good evidence?
(b) Evaluate the prediction: assuming the manufacturers claim inaccurate, is someone in the
cafeteria diluting the vinegar? Include an accuracy calculation (percent error) in your
evaluation.

Determining Empirical Formula of Magnesium Oxide


Abstract
Early chemists had a great deal of qualitative information about the known elements and their
compounds. To formulate theories of atomic structure, however, quantitative data were needed.
Chemists analyzed many compounds to determine not only which elements were present, but in
what amounts by mass. From these experiments, the percentage composition and the number of
atoms in a compound could be found. This information gives the formula of a compound.
Purpose
1. To prepare a binary compound.
2. To find its percentage composition by mass.
3. To determine the formula of the compound.
Materials
crucible and lid
crucible tongs
clay triangle
ring stand
ring clamp

Bunsen burner
scissors
balance, 0.01g
Ceramic fibre pad
15 cm of magnesium
ribbon

Procedure
1. Prepare for the experiment by putting on eye protection and a protective apron.
2. Assemble the equipment as shown in figure 1.
3. Heat a clean crucible and lid until the crucible becomes red, cool it, and determine its mass to
an accuracy of 0.01 g.
4. Cut the magnesium ribbon into small pieces. Place the small pieces into the crucible and cover
it with a lid. Determine the total mass.
5. Place the crucible lid over the contents. The lid should be left slightly ajar. Do not let any of the
solid product escape from the crucible.
6. Begin by gently heating the crucible until the reaction starts. After the reaction has stopped,
heat the crucible strongly for several minutes. Do not stop heating until your crucible has been
checked by your teacher.

Figure 1 Apparatus Set Up

7. Allow the crucible to cool. When the crucible has cooled, remove the lid and add a few drops
of water to the reaction product. Replace the lid as before, and reheat for several minutes.
8. Allow the crucible to cool. Determine the mass of the crucible, lid, and contents.
9. Examine the contents of the crucible and note any changes that have occurred.

Observations
Table 1 Measured Masses
Measured Object

Mass (g)

Mass of Crucible and lid


Mass of Metal, Crucible, and Lid
Mass of Magnesium
Mass of Crucible and Lid
(previously measured)
Mass of Product, Crucible, and Lid
(1st heating)
Mass of Product (2nd heating)
Mass of Product (3rd heating)
Mass of Magnesium
Increase in Mass
Mass of the Element that Combined
with the magnesium

Analysis
1. Calculate the following:
a. The mass of the magnesium used, and the mass of the compound formed.
b. The mass of the element that combined with the magnesium. Use the information in your
data table to do this.
2. Calculate the percentage composition by mass of the compound.
3. Consider a 100 g sample of the compound. Calculate the number of metal atoms present. Also
calculate the number of atoms of the other element in the compound. These numbers are
expressed as metal and oxygen.
4. Compare the number of metal atoms to the number of oxygen atoms. Write the empirical
formula for the compound.

Questions
1. What observations suggest that the formation of a compound is a chemical change rather
than a physical one?
2. Why did the compound have a greater mass than the original metal? Write a word
equation indicating the process that took place.
3. Why was it not necessary to determine the mass of the oxygen before the reaction?
4. Why was the crucible heated strongly after the reaction had apparently been completed?
5. a. What did you notice after the water was added to the reaction product in step 7? b.
What could account for this observation?
6. Compare your numerical results with four other groups. Are they the same? If not,
suggest possible reasons for any differences. How might this experiment be improved to
obtain more accurate results?
Conclusion
1. State the compounds percent composition by mass.
2. State the formula of the compound formed.

Percent Composition of a Hydrate


The concept of percent composition is often used to determine how many grams of an element
might be produced when a compound is decomposed, or how many grams of an element is
necessary to produce a given quantity of compound (in grams). By using the mole relationship to
get mass/number conversion factors, it is possible to determine the number of moles of water
present per mole of copper sulfate.
A. Definition

Hydrates are compounds having water incorporated within the crystal structure in specific
whole number ratios.
The bonds holding the water are weak bonds and are easily broken when heated.

Today you will determine both the percent of water present in a hydrate copper (II) sulfate
(CuSO4 nH2O) and n the number of moles of water molecules present per mole of CuSO4.
B. Calculating Percent Composition

The percent composition values can be used to calculate the number of grams of an element in a
given mass of compound.

Example II:

Calculate the number of grams of oxygen that would be present in a 4.00 gram
sample of phosphoric acid, H3PO4.
Solution:
From the previous example, 65.3% of phosphoric acid (H3PO4) is oxygen by mass. This means
that there are 65.3 grams of O in 100grams of the compound phosphoric acid.Therefore:

Finding the mass percent water in a hydrate is very similar. The only difference is the
replacement of the element mass by the mass of water (H2O).
Example III: The formula of a hydrate of barium chloride is BaCl2 2H2O. Find the mass
percent water in this hydrate.
Solution:

C. Experimental Considerations
In this experiment, you will be heating a hydrate of copper (II) sulfate (CuSO4 nH2O) to drive
off the water. Masses are taken before heating to determine the mass of the original sample (the
hydrate) and after heating to determine the mass of copper (II) sulfate (CuSO4) remaining. The
difference between these two masses is equal to the mass of the water lost. Heating time and
temperature are critically important for this experiment. If not enough heat is applied, some
water will remain attached to the copper sulfate producing a low calculated mass percent water
for the hydrate. If too much heat is applied, the anhydrous copper (II) sulfate (CuSO4), which has
a grayish white color, can be decomposed to copper (II) sulfide, a black colored compound.

D. Experimental Procedure

After you have washed the crucible and lid, use only tongs (not your hands) to handle them
1. Place a clean, empty crucible with lid in a clay triangle on a ring stand (as shown in diagram). Tilt
the lid so that it is slightly ajar, then heat strongly (bottom of crucible should turn red) for about 3
minutes. Turn off the Bunsen burner, and use tongs to close the lid so that water from the air does
not get inside the dry crucible. Allow the crucible and lid to cool (this should take 5 minutes).
2. Using tongs, transfer the crucible and lid (still closed) to a wire gauze and carry them to the
balance. Its okay if you need to remove the lid momentarily to transfer the crucible & lid
separately to the wire gauze. Mass the crucible and lid (together) carefully to the nearest 0.01g
and record the mass in the Data Table provided.
3. Add approximately 2.5- 3.5g of the copper (II) sulfate hydrate to the crucible and mass the
crucible with the hydrate and the lid again to the nearest 0.01g. Record the mass in the Data Table.
4. With the lid slightly ajar, heat the crucible gently (crucible should NOT glow red; use the top of
the outer flame, not the inner flame) for about 12 minutes. Turn off the Bunsen burner and use
tongs to close the lid. Allow the crucible with sample and closed lid to cool for 5 minutes, then
mass to the nearest 0.01g, recording the mass in the Data Table. During the time you are cooling
the sample and crucible you can be working on the Exercise questions at the end of this
experiment.
5. Reheat the sample for 2-3 minutes (with lid slightly ajar), cool (with lid closed) and mass again.
This should be repeated until the successive masses are constant within 0.03g. When the masses
are constant, record the lowest mass as the final mass.
Waste Disposal: Place compound remaining in your crucible in the jar labeled Copper Sulfate
Collection. Note the color of the solid closest to the crucible bottom:

Figure1: Apparatus set up

Observations:
Table1: Measuring the mass of hydrate/anhydrous compounds
1.

Mass of empty, dry crucible and lid (after heating


& cooling)

2.

Mass of lid, crucible and hydrate (before heating


the sample)

3.

Mass of hydrate (original sample)

4.

Mass of crucible, lid, and dehydrated sample:


after first heating & cooling
after second heating & cooling
after third heating & cooling (if needed)
final mass

5.

Mass of the water driven off

6.

Mass percent water in the hydrate (show


calculations below)

E. Analysis
1. How many moles of copper (II) sulfate (CuSO4) and how many moles of water did you

have in your original sample? Hint: Convert each mass using molar mass (g/mol

2. Examine the formula for the hydrate: CuSO4 n H2O. Notice that n is the molar

ratio of water to copper sulfate. Find the numerical value for n in this sample (use
your numbers from part a above). Hint: what does molar ratio of water to copper
sulfate mean? Write it as a fraction then solve it, since n = the molar ratio of water
to copper sulfate.

3. The actual mass percent of water in the hydrated copper (II) sulfate compound should

have been 36.1%. Compare this value to the experimental percentage you obtained.
Hint: how do you quantitatively compare an experimental value to an actual value?

4. In the experiment involving hydrated copper sulfate, overheating causes a high calculated

percent value for water. Why is the high reading obtained? Hint: Overheating causes
copper (II) sulfate, CuSO4 to turn into copper (II) sulfide, CuS. What is lost from the
CuSO4 in this process? Where does it go?

5. What experimental evidence would you have to indicate you inadvertently overheated

the hydrated copper sulfate compound? Hint: Re-read the Experimental


Considerations section.

F. Exercise Questions
6. Determine the mass percent of each element present in CaCO3.

7. Determine the number of grams of Na present in 4.0g of NaOH.

8. Calculate the mass percent water in MgSO4 2 H2O.

Reference:
Canham, G., Damji, S., Goering - Boone, U., Bloch, M., & Bloch, P. (2002).
Chapter 7: Reactions in Solution. In Addison Wesley chemistry 11 (p. 310). Toronto:
AddisonWesley.
Clancy, C., Mustoe, F., Doran, T., Ivanco, J., Ghazariansteja, A., & Jansen, M.
(2001). Chapter 10: Acids and Bases. In McGraw-Hill Ryerson chemistry 11 (pp. 399 404). Whitby, Ont.: McGraw-Hill Ryerson.
Jenkins, F., Van Kessel, H., Davis, L., Thomas, O., Tompkins, D., & Thomas, P.
(2002). Chapter 8: Acids and Bases. In Nelson chemistry 11 (pp. 398 - 400). Toronto:
Nelson Thomson Learning.
The Titration of Acetic Acid in Vinegar. (n.d.). In General Chemistry Laboratory
(pp. 5 - 8). Http://infohost.nmt.edu/~jaltig/Vinegar.pdf.
Henderson, D. (2010). Experiment 1: Acid, Base Titration. In Analytical
Chemistry Lab Manual (pp. 26 - 29). Toronto: Trinity College
Note: Determine Empirical Formula of Magnesium Oxide and Percent Composition of a
Hydrate are two labs that I was able to perform with my students during placement, and I
do not remember from where I got them.