3 AUDIOBOOK COLLECTIONS

6 BOOK COLLECTIONS
 Honors Chemistry Lab Fall

By: Mary McHale

Online: <http://cnx.org/content/col10456/1.16>

This selection and arrangement of content as a collection is copyrighted by Mary McHale.

It is licensed under the Creative Commons Attribution License: http://creativecommons.org/licenses/by/2.0/
Collection structure revised: 2007/11/15
For copyright and attribution information for the modules contained in this collection, see the "Attributions" section at the end of the
collection.
 Honors Chemistry Lab Fall

Table of Contents

Chapter 1. Initial Lab: Avogradro and All That

1.1.
Chapter 2. Stoichiometry: Laws to Moles to Molarity
2.1.
Experiment 2: Stoichiometry: Laws to Moles to Molarity
Objective
Grading
Before Coming to Lab..
Introduction
Titration Calculations:
Example:
Experimental
Materials List
Procedure
Part 1
Materials List
Part 2
Pre-Lab 2: Stoichiometry
Report 2: Stoichiometry
Part 1
Data Table
Discussion Questions
Part 2
Chapter 3. VSEPR: Molecular Shapes and Isomerism
3.1.
Grading
Chapter 4. Beer's Law and Data Analysis
4.1.
Beer’s Law and Data Analysis
Objectives
Grading
Before coming to lab…
Introduction
Extracting Quantitative Information
Experimental Procedure
Analysis
PreLab: Spectrophotometry and Data Analysis – Beer’s Law
 Questions:
Chapter 5. Hydrogen and Fuel Cells
5.1.
Hydrogen and Fuel Cells Experiment
Objective
Grading
Before Coming to Lab…
Introduction
The Chemistry of a Fuel Cell
Experimental
Caution!!! Plastic can burn.
Pre-Lab: (Total 10 Points)
Report (80 points)
Chapter 6. The Best Table in the World
6.1.
The Best Table in the World!
Objective
Grading
Background Information
Introduction
Relative Reactivity of Metals and the Activity Series
Procedure
I. Activity Series
Part 1. Reactions of Metals with Water
Part 2. Reactions of Metals with HCl
Part 3. Reactions of Metals with Other Metal Ions
Part 4. Flame Tests
One station set up that all sections will rotate through
Pre-Lab 5: The Best Table in the World!
Report 5: The Best Table in the World!
I. Activity Series
Part 1. Reactions of Metals with Water
Part 2. Reactions with HCl
Part 3. Reactions with Other Metal Ions
Part 4. Flame Tests
Chapter 7. Bonding 07
7.1.
Lab 5: Bonding 07
Objective
Grading
Background Information
Experimental Procedure
Part I. Predicting bond type through electronegativity differences.
 Part II. Weak and strong electrolytes
Chemicals
Instructions for MicroLab Conductivity Experiment
Part III. Electrolyte strength and reaction rate
Chemicals
Part IV. Chemical reactions
Chemicals
Pre-Lab 5: Bonding 07
(Total 10 Points)
Part I. Bonding of chemicals in solution
Report 5: Bonding 07
Part I. Predicting bond type through electronegativity differences.
Part II. Weak and strong electrolytes
Part III. Electrolyte strength and reaction rate
Part IV. Chemical reactions
Chapter 8. Solid State and Superconductors
8.1.
Solid State Structures and Superconductors
Objectives
Grading
Before coming to lab:
Introduction
Stoichiometry
Binding forces in a crystal
Close-packing
Packing of more than one type of ion (binary compounds) in a crystal
lattice
Coordination number and interstitial sites
Synthesis of solid state materials
X-ray crystallography

Superconductors
Solid State Model Kits
Use of the Solid State Model Kit:
Working groups and teams
Experimental Procedure

2. Cubic Cells
Team A
Group 2. Extended Structure
4. Interstitial sites and coordination number (CN)
Team A
5. Ionic Compounds
 Team C
Fluorite: Calcium fluoride
Team D
Lithium Nitride
· Use the L template and insert 6 rods in the parallelogram portion of the
dotted lines.
· Construct the pattern shown below. Be sure to include a z=1 layer. 1 is a
green sphere while 1 and 2 are blue spheres. The 0 indicates a 4.0 mm
spacer tube; the 2 is an 18.6 mm spacer.
Teams E and F
Zinc Blende and Wurtzite: Zinc Sulfide
Pre-Lab: Solid State and Superconductors
(Total 10 Points)
Report: Solid State and Superconductors
A. Simple Cubic Unit Cells or Primitive Cubic Unit Cells (P)
B. Body-Centered Cubic (BCC) Structure
C. The Face Centered Cubic (FCC) Unit Cell
a. Fill out the following table for a FCC unit cell.
IV.Ionic Solids
Chapter 9. Organic Reactions
9.1.
Organic Reactions
Objectives
Grading
Introduction
EXPERIMENTAL PROCEDURE
Synthesis of esters
Oxidation of an alcohol with acidified potassium dichromate(VI) solution
Oxidation of an alcohol with acidified potassium permanganate (VII)
solution
Saponification of a vegetable oil
Pre-Lab: Introductory Organic Reactions
(Total 25 Points)
Report: Organic Reactions
Observations:
Synthesis of esters
Oxidation of an alcohol with acidified potassium dichromate(VI) solution.
Oxidation of an alcohol with acidified potassium permanganate (VII) solution

Saponification of a vegetable oil

Chapter 10. Transition Metals
10.1.
Transitions Metals: Synthesis of an Inorganic Compound (trans-
 dinitrobis(ethylenediamine)cobalt(III) nitrate)
Objectives
Grading
Introduction
Stereochemistry
Experimental Procedure
Pre-Lab: Transition Metals
(Total 10 Points)
Report: Transition Metals
1. Synthesis

a. Observations

b. Questions
Chapter 11. Physical Properties of Gases
11.1.
Physical Properties of Gases
Objectives
Grading
Introduction
Experimental Procedure
Diffusion:
Gas Laws in a Soda Can:
Balloon in liquid nitrogen:
Tygon tube in liquid nitrogen:
Balloon in a flask:
Cartesian diver:
The Egg:
Expanding balloon:
Bonus 2 points:
Pre-Lab: Physical Properties of Gases
(Total 10 Points)
Report: Physical Properties of Gases
(Total 80 Points)
Index
 Chapter 1. Initial Lab: Avogradro and All That

Initial Lab: Avogadro and All ThatExperiment 1

Objective

The purpose of this laboratory exercise is to help you familiarize yourself with the layout of the
laboratory including safety aids and the equipment that you will be using this year.

Then, to make an order-of-magnitude estimate of the size of a carbon atom and of the number
of atoms in a mole of carbon based on simple assumptions about the spreading of a thin film of
stearic acid on a water surface

Grading

Pre-lab – not required for the first lab

Lab Report (90%)

TA points (10%)

Before coming to lab……

Read the following:

Lab instructions

Background Information

Concepts of the experiment

Print out the lab instructions and report form.

You may fill out the lab survey, due at the beginning of the lab, for extra credit if you wish.

Read and sign the equipment responsibility form and the safety rules, email Ms Duval at
[email protected] to confirm completing this requirement by noon on August 31st

Introduction

Since chemistry is an empirical (experimental) quantitative science, most of the experiments you
will do involve measurement. Over the two semesters, you will measure many different types of
quantities – temperature, pH, absorbance, etc. – but the most common quantity you will measure
will be the amount of a substance. The amount may be measured by (1) weight or mass (grams),
(2) volume (milliliters or liters), or (3) determining the number of moles. In this experiment we
will review the methods of measuring mass and volume and the calculations whereby number of
moles are determined.

Experimental Procedure

We will start in the amphitheater of DBH (above DBH 180) for demonstrations: oxygen, hydrogen
and a mixture of the two in balloons and more besides.

Mandatory Safety talk by Kathryn Cavender, Director of Environmental Health and Safety at Rice.

1. Identification of Apparatus

On your benches, there are a number of different pieces of common equipment. With your TA's
help, identify each and sketch - I know this may sound a trivial exercise but it is necessary so that
we are all on the same page.

1. beaker

2. erlenmeyer flask

3. graduated (measuring) cylinder

4. pipette

5. burette

6. Bunsen burner

7. test tube

8. boiling tube

9. watch glass

2. Balance Use

In these general chemistry laboratories, we only use easy-to-read electronic balances – saving you
a lot of time and the TA’s a lot of headaches. However, it is important that you become adept at
the use of them.

Three aspects of a balance are important:

1. The on/off switch. This is either on the front of the balance or on the back.

2. The "Zero" or "Tare" button. This resets the reading to zero.

2. The "Zero" or "Tare" button. This resets the reading to zero.

3. CLEANLINESS. Before and after using a balance, ensure that the entire assembly is spotless.
Dirt on the weighing pan can cause erroneous measurements, and chemicals inside the
machine can damage it.

4. Turn the balance on.

5. After the display reads zero, place a piece of weighing paper on the pan.

6. Read and record the mass. (2)

7. With a spatula, weigh approximately 0.2 g of a solid, common salt NaCl, the excess salt is
discarded, since returning the excess salt may contaminate the rest of the salt - in this exercise,
this is not a big deal but in strict analytical procedures it is.

8. Record the mass (1). To determine how much solid you actually have, simply subtract the
mass of the weighing paper(2) from the mass of the weighing paper and solid (1). Record this
mass (3).You have just determined the mass of an "unknown amount of solid."

9. Now place another piece of weighing paper on the balance and press the Zero or Tare button
then weigh out approximately 0.2 g of the salt (4). Thus, the zero/tare button eliminates the
need for subtraction.

3. Measuring the volume of liquids

When working with liquids, we usually describe the quantity of the liquid in terms of volume,
usual units being milliliters (mL). We use three types of glassware to measure volume – (1)
burette, (2) volumetric pipette, and (3) graduated cylinder.

Examine each piece of equipment. Note that the sides of each are graduated for the graduated
cylinder and the burette. You can read each to the accuracy of half a division.

Put some water into the graduated cylinder. Bend down and examine the side of the water level.
Note that it has a "curved shape." This is due to the water clinging to the glass sides and is
called the meniscus. When reading any liquid level, use the center of the meniscus as your
reference point.

Graduated cylinder

1. Look at the graduations on the side of the cylinder. Note that they go from 0 on the bottom and
increase upwards. Thus, to get the mass of 10 mL of a liquid from a graduated cylinder, do the
following:

2. Add water up to the 10 mL line as accurately as possible.

3. Dry a small beaker and weigh it (2).

3. Dry a small beaker and weigh it (2).

4. Pour the 10 mL of water from the cylinder into the beaker. Reweigh (1).

5. Subtract the appropriate values to get the weight of the water (3).

Pipette

1. You may find either that 0 is at the spout end or at the top of the pipette. You should be aware
of how these graduations go when using each pipette. Thus, to get the mass of 10 mL of a
liquid from a pipette, do the following:

2. Half-fill a beaker with water.

3. Squeeze the pipette bulb and attach to the top of the pipette. Put the spout of the pipette under
water and release the bulb. It should expand, drawing the water into the pipette, do not let the
water be drawn into the bulb.

4. When the water level is past the last graduation, remove the bulb, replace with your finger, and
then remove the pipette from the water.

5. Removal of your finger will allow liquid to leave the pipette. Always run some liquid into a
waste container in order to leave the level at an easy-to-read mark.

6. Add 10 mL of water to a pre-weighed dry beaker (5).

7. Weigh (4).

8. Subtract to get the weight of the water (6).

Burette

1. Examine the graduations. Note that 0 is at the top.

2. Using a funnel, add about 10 mL of water. To do this, first lower the burette so that the top is
easy to reach.

3. Run a little water from the burette into a waste container. Then turn the burette upside down
and allow the rest of the water to run into the container (you will have to open the top to
equalize the pressure).

4. You have just "rinsed your burette." This should be done every time before using a burette –
first rinse with water, then repeat the process using whatever liquid is needed in the
experiment.

5. Fill the burette to any convenient level (half-way is fine). It is a good technique to "overfill"
 and then allow liquid to run into a waste container until you reach the appropriate level so that
you fill the space from the top to the tip of the burette.

6. Dry a beaker and weigh (8).

7. Add 10 mL of water to a pre-weighed dry beaker (7).

8. Subtract to get the weight of the water (9).

4. Estimation of Avogadro's number

Briefly, as a group with your TA, you will make an approximate (order of magnitude) estimate of
Avogadro's number by determining the amount of stearic acid that it takes to form a single layer
(called a monolayer) on the surface of water. By making simple assumptions about the way the
stearic acid molecules pack together to form the monolayer, we can determine its thickness, and
from that thickness we can estimate the size of a carbon atom. Knowing the size of a carbon atom,
we can compute its volume; and if we know the volume occupied by a mole of carbon (in the form
of a diamond), we can divide the volume of a mole of carbon by the volume of an atom of carbon
to get an estimate of Avogadro's number.

Procedure

Special Supplies: 14 cm watch glass; cm ruler; polyethylene transfer pipets; 1-mL syringes; pure
distilled water free of surface active materials; disposable rubber gloves (for cleaning own watch
glasses in 0.1 M NaOH in 50:50 methanol/water): 13 X 100 mm test tubes with rubber stoppers to
fit.

Chemicals: pure hexane, 0.108 g/L stearic acid (purified grade) solution in hexane. 0.1 M NaOH
in 50:50 methanol/water used for washing the watch glasses.

SAFETY PRECAUTIONS: Hexane is flammable! There must be no open flames in the laboratory
while hexane is being used.

WASTE COLLECTION: At the end of the experiment, unused hexane solvent and stearic acid in
hexane solution should be placed in a waste container, marked "Waste hexane/stearic acid solution
in hexane."

Measurement of the volume of stearic acid solution required to cover the water surface

Your TA will do this as a group demonstration:

1. Using a transfer pipette, obtain about 3-4 mL 0.108 g/L stearic acid solution in hexane in a
clean, dry 13 X 100 mm test tube. Keep the tube corked when not in use.

2. Fill the clean watch glass to brim with deionized water. One recommended way to do this is to
 set up your 25 mL burette on a ring stand. Wash and drain the burette with deionized water.
(the deionized water comes from the white handled spouts at each sink)

3. In a freshly cleaned and rinsed beaker, obtain more distilled water and fill the burette. Place
your watch glass directly under the burette (about 1 inch or less from the tip) and dispense the
water until the entire watch glass is full. You may have to refill the burette 4 or 5 times to do
this. With careful dispensing, the surface tension of the water should allow you to fill the
entire watch glass with relative ease.

4. Carefully measure the diameter of the water surface with a centimeter ruler. It should be close
to 14 cm, + or - a couple of millimeters. Next, rinse and fill your 1 mL syringe with stearic
acid solution, taking care to eliminate bubbles in the solution inside the syringe.

5. Read and record the initial volume of the syringe (1 mL is always a good place to start.)

6. Then add the stearic acid solution drop by drop to the water surface. Initially, the solution will
spread across the entire surface, and it will continue to do so until a complete monolayer of
stearic acid has been formed. If your first few drops do not spread and evaporate quickly,
either your water or watch glass is still dirty. As this point is approached, the spreading will
become slower and slower, until finally a drop will not spread out but will instead sit on the
surface of the water (looking like a little contact lens). If this "lens" persists for at least 30 s,
you can safely conclude that you have added 1 drop more than is required to form a complete
monolayer.

7. Now, read and record the final volume reading of the syringe.Takes 10 min

8. Thoroughly clean the watch glass (or get another one), and repeat the experiment. Repeat until
the results agree to within 2 or 3 drops (0.04 ml).

When you have completed all of your measurements, rinse your syringe with pure hexane, and
dispose of all the hexane-containing solutions in the waste collection bottle provided.

Calculation Of Avogadro's Number

The calculation proceeds in several steps.

We calculate the volume of stearic acid solution in hexane required to deliver enough stearic
acid to form a monolayer.

All of the hexane evaporates, leaving only the thin monolayer film of stearic acid, so we next
calculate the actual mass of pure stearic acid in the monolayer.

We calculate the thickness of the stearic acid monolayer, using the known density of stearic
acid and the area of the monolayer.

Assuming the stearic acid molecules are stacked on end and are tightly packed, and knowing
 Assuming the stearic acid molecules are stacked on end and are tightly packed, and knowing
that there are 18 carbon atoms linked together in the stearic acid molecule, calculate the
diameter and volume of a carbon atom.

Calculate the volume of a mole of carbon atoms in diamond; divide the molar volume of carbon
(diamond) by the volume of a single carbon atom to obtain an estimate of Avogadro's number.
Remember that the units of Avogadro’s number are mol-1, so you can use unit analysis to
check your answer.

Initial Lab: Avogadro and All ThatReport 1

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Demonstrations:

Balloons:

1. Oxygen

1. Hydrogen

2. Mixture of Hydrogen and Oxygen with relevant equation: H2 + O2→

Thermite:

Include description and relevant equation: Fe2 O3 + Al →

Dry Ice and Magnesium:

Include description and relevant equation: MgO + C →

1. Identification of Apparatus

1. beaker
1. erlenmeyer flask

1. graduated (measuring) cylinder

1. pipette

1. burette

1. Bunsen burner

1. test tube

2. watch glass

2. Balance Use

1. Mass of weighing paper and solid, ________ g

2. Mass of weighing paper, __________ g

3. Mass of solid, ___________g

4. Mass of solid on tared weighing paper ____________g

3. Measuring the volume of a liquid

1. Mass of 50 mL beaker and water, g ______________

2. Mass of 50 mL beaker, g ______________________

3. Mass of water from graduated cylinder, g___________

4. Mass of 50 mL beaker and water, g ______________

5. Mass of 50 mL beaker, g ______________________

6. Mass of water from pipette, g ____________________

7. Mass of 50 mL beaker and water, g ______________

8. Mass of 50 mL beaker, g ______________________

9. Mass of water from burette, g ____________________

From a consideration of the masses of water measured above, and given that the density of water
is 1 g/mL, decide on an order of which is the most accurate method of volume measurement –
measuring cylinder, pipette, or burette with (1) being the most accurate?

(1)

(2)

(3)

How precisely could each of the apparatus used be read?

(1) measuring cylinder

(2) pipette

(3) burette

4. Estimation of Avogadro's Number

Measurement of the volume of stearic acid solution required to cover the water surface

Table 1.1.

Trial 1 Trial 2

Record the diameter of the water surface ___________________ ___________________

Record the volume of stearic acid solution

___________________ ___________________
required to cover the surface

Record the concentration of the stearic acid

___________________ ___________________
solution
Calculation Of Avogadro's Number

a. Calculation of the thickness of a monolayer of stearic acid

Table 1.2.

Trial 1 Trial 2

From your data, the volume of stearic acid

___________________ ___________________
solution required to form a monolayer was

Calculate the mass of stearic acid contained in

that volume of stearic acid solution (the
___________________ ___________________
concentration in grams per liter will be given
to you)

Calculate the volume, V, of pure stearic acid

in the monolayer on the water surface. You
___________________ ___________________
will need the density of solid stearic acid,
which is 0.85 g/ml (or g/cm3).

Calculate the area of the monolayer (A = πr2, r

___________________ ___________________
is the radius of the water surface)

Calculate the thickness of the monolayer (t =

___________________ ___________________
Volume/Area)

b. Estimation of the size and volume of a carbon atom

Table 1.3.

Trial 1 Trial 2

A stearic acid molecule consists of 18 carbon

atoms linked together. Assuming that the
thickness, t, of a monolayer is equal to the ___________________ ___________________
length of the stearic acid molecule, calculate
the size of a carbon atom, s = t/18
Assuming that a carbon atom is a little cube,
calculate the volume of a carbon atom, volume ___________________ ___________________
= s3

c. Calculation of the volume of a mole of carbon atoms

Table 1.4.

Trial 1 Trial 2

Calculate the molar volume of carbon

(diamond) by using the density of
______________________________ _______________
diamond (3.51g/cm3) and the atomic
mass of a mole of carbon

Is the volume of a mole of diamond

the same as the actual volume of a ______________________________ _______________
mole of carbon atoms?

d. Calculation of the volume of a mole of carbon (diamond) volume of a single carbon atom
(Avogadro's number)

Table 1.5.

Trial 1 Trial 2

Calculate Avogado's number (NA)

from the appropriate ratio of _________________________________ _____________
volumes

Calculate the average value of NA

_________________________________ _____________
from your results

Express your results as a number

1023. Are you within a power of 10 ________________________________ _____________
of the accepted value of 6.02 1023?

Solutions
 Chapter 2. Stoichiometry: Laws to Moles to Molarity

Experiment 2: Stoichiometry: Laws to Moles to Molarity

Objective

To determine the mass of a product of a chemical reaction

To make a solution of assigned molarity – your accuracy will be tested by your TA by titration!

Grading

Pre-lab (10%)

Lab Report (80%)

TA points (10%)

Before Coming to Lab..

Read the lab instructions

Complete the pre-lab, due at the beginning of the lab

Introduction

The word stoichiometry derives from two Greek words: stoicheion (meaning "element") and
metron (meaning "measure"). Stoichiometry deals with calculations about the masses (sometimes
volumes) of reactants and products involved in a chemical reaction. Consequently, it is a very
mathematical part of chemistry.

In the first part of this lab, sodium bicarbonate is reacted with an excess of hydrochloric acid.

NaHCO 3 ( s ) + HCl ( aq ) → NaCl ( aq ) + CO 2 ( g ) + H 2 O

By measuring the mass of NaHCO3 and balancing the equation (above), the mass of NaCl
expected to be produced can be calculated and then checked experimentally. Then, the actual
amount of NaCl produced can be compared to the predicted amount.

This process includes molar ratios, molar masses, balancing and interpreting equations, and
conversions between grams and moles and can be summarized as follows:

1. Check that the chemical equation is correctly balanced.

2. Using the molar mass of the given substance, convert the mass given in the problem to moles.

3. Construct a molar proportion (two molar ratios set equal to each other). Use it to convert to
moles of the unknown.

4. Using the molar mass of the unknown substance, convert the moles just calculated to mass.

In the second part of this lab, since a great deal of chemistry is done with solutions, a solution will
be prepared of allocated molarity. Molarity, or more correctly molar concentration, is defined to
be the number of moles of solute divided by the number of liters of solution:

with units of [mole/L]. However molar concentration depends on the temperature so a higher
temperature would result in an increased volume with a consequential decrease in molar
concentration. This can be a significant source of error, of the same order as the error in the
volume measurements of a burette, when the temperature increases more than 5 º C.

Steps to preparing a solution of a certain concentration:

1. First need to know the formula for the solute, e.g. potassium chromate: K2CrO4.

2. Need the molecular weight of the solute: by adding up the atomic weights of potassium,
chromium and oxygen: 39.10, 52.00 and 16.00 in the correct ratios:

3. 2 × 39 . 1, 52 . 0 and 4 × 16 . 00 = 194 . 2g/mole .

4. Then the volume of solution, usually deionised water: e.g. for one liter of solution use a 1000
mL volumetric flask. So a 1M solution would require 194.2g of solid K2CrO4 in 1 L, 0.1M
19.42g of solid K2CrO4 and so on.

5. Remember to ensure that all the solute is dissolved before finally filling to the mark on the
volumetric flask. If there is any undissolved solute present in the solution, the water level will
go down slightly below the mark, since the volume occupied by the solute differs from the
actual volume it contributes to the solution once it is dissolved.

Your teaching assistant will check the accuracy of the solution that you have made by titration,
which is a method of quantitatively determining the concentration of a solution. A standard
solution (known concentration) is slowly added from a burette to a solution of the analyte
(unknown concentration – your solution) until the reaction between them is judged to be complete
equivalence point). In colorimetric titration, some indicator must be used to locate the
equivalence point. One example is the addition of acid to base using phenolphthalein (indicator) to
turn a pink solution colorless in order to determine the concentration of unknown acids and bases.
Record your TAs value of the molarity of your solution on your report form along with your
percent error.

Figure 2.1.

Figure 1: Reading the Burette

When an acid is neutralized by a base, since there is stoichiometrically equal amounts of acid and
base and the pH = 7, it is possible to accurately determine the concentration of either the acid or
base solution. Since:

Moles of a substance = Concentration of solution (moles/L) x Volume (L)

We can calculate the concentration of the acid or base in the solution using:

Titration Calculations:

Step 1:Balance the neutralization equation. Determine Balance of Acid and Base.

Step 2:Determine what information is given.

Step 3:Determine what information is required.

Step 4:Solve using the equation below.

Β b × C a × V a = Βa × C b × V b
Example:

Calculate the concentration of a nitric acid solution HNO3 if a 20 ml sample of the acid required
an average volume of 55 ml of a 0.047 mol/l solution of Ba OH 2 to reach the endpoint of the
titration.

Step 1: 2HNO3+Ba OH 2→Ba NO3 2+2H2OBalance Base = 1Balance Acid = 2

Step 2:Given informationVolume Acid = 20 mlVolume Base (average) = 55 ml Concentration of

Base = 0.047 mol/l

Step 3: Required informationConcentration of AcidStep 4:Solve using the equation.

Βb×Ca×Va=Βa×Cb×Vb1×Ca×20ml=2×0.047mol/1×55ml Ca = 0.2585 mol/l ( considering
significant figures 0.26 mol/l)

Experimental

Materials List

sodium bicarbonate NaHCO3

3M hydrochloric acid (HCl) solution

Procedure

Part 1

1. Weigh an empty 150-mL beaker on the electronic balance. Record this value in your data
table.

2. Remove the beaker from the balance and add one spoonful of sodium bicarbonate
(approximately 5 g). Re-weigh and record this value.

3. Pour approximately 20 mL of 3M hydrochloric acid into a 100-mL beaker. Rest a Pasteur

pipette in the beaker.

4. Add 3 drops of acid to the NaHCO3beaker, moving the pipette so that no drops land on each
other. The key point is to spread out the adding of acid so as to hold all splatter within the
walls of the beaker.

5. Continue to add acid slowly drop by drop. As liquid begins to build up, gently swirl the beaker.
 This is done to make sure any unreacted acid reaches any unreacted sodium bicarbonate. Do
not add acid while swirling.

6. Stop adding the hydrochloric acid when all bubbling has ceased. So that the minimum amount
of HCl has reacted with all of the sodium bicarbonate. Check when all the bubbling has ceased,
by swirling the beaker and to ensure that there is no more bubbling. When all the bubbling has
ceased, add one drop more of acid and swirl.

7. Weigh the beaker and contents, record.

8. Using a microwave oven, dry to constant weigh, initially for 1 min, when there is plenty of
solution, and then 10 second intervals thereafter. Measure weight to the nearest milligram.

Materials List

100 mls volumetric flask

3M hydrochloric acid (HCl) solution

sodium bicarbonate NaHCO3

methyl orange indicator

Part 2

1. Ask you TA for your assigned molarity – it will range from 0.7 M to 1.2 M.

2. First need to know the formula for the solute.

3. Need the molecular weight of the solute in g/mole.

4. The volume of solution, 100 mLs.

5. Remember to ensure that all the solute is dissolved before finally filling with deionised water
to the mark on the volumetric flask.

6. Take your solution to your TA to check the molarity by titration, record value on your report
form and your percent error.

Pre-Lab 2: Stoichiometry
(Total 10 points)
Click here to print the Pre-Lab Note: In preparing this Pre-Lab you are free to use references and
consult with others. However, you may not copy from other students’ work (including your
laboratory partner) or misrepresent your own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Circle the correct answer:

1) Which one of the following is a correct expression for molarity?

A) mol solute/L solvent

B) mol solute/mL solvent

C) mmol solute/mL solution

D) mol solute/kg solvent

E) μmol solute/L solution

2) What is the concentration (M) of KCl in a solution made by mixing 25.0 mL of 0.100 M KCl
with 50.0 mL of 0.100 M KCl?

A) 0.100

B) 0.0500

C) 0.0333

D) 0.0250

E) 125

3) How many grams of CH3OH must be added to water to prepare 150 mL of a solution that is 2.0
M CH3OH?

A) 9.6 × 103

B) 4.3 × 102

C) 2.4

D) 9.6
E) 4.3

4) The concentration of species in 500 mL of a 2.104 M solution of sodium sulfate is __________

M sodium ion and __________ M sulfate ion.

A) 2.104, 1.052

B) 2.104, 2.104

C) 2.104, 4.208

D) 1.052, 1.052

E) 4.208, 2.104

5) Oxalic acid is a diprotic acid. Calculate the percent of oxalic acid H2C2O4 in a solid given that a
0.7984 g sample of that solid required 37.98 mL of 0.2283 M NaOH for neutralization.

A) 48.89

B) 97.78

C) 28.59

D) 1.086

E) 22.83

6) A 31.5 mL aliquot of H2SO4(aq) of unknown concentration was titrated with 0.0134 M NaOH
(aq). It took 23.9 mL of the base to reach the endpoint of the titration. The concentration (M) of
the acid was __________.

A) 0.0102

B) 0.0051

C) 0.0204

D) 0.102

E) 0.227

7) What are the respective concentrations (M) of Fe3+ and I− afforded by dissolving 0.200 mol
FeI3 in water and diluting to 725 mL?
A) 0.276 and 0.828

B) 0.828 and 0.276

C) 0.276 and 0.276

D) 0.145 and 0.435

E) 0.145 and 0.0483

8) A 36.3 mL aliquot of 0.0529 M H2SO4(aq) is to be titrated with 0.0411 M NaOH (aq). What
volume (mL) of base will it take to reach the equivalence point?

A) 93.6

B) 46.8

C) 187

D) 1.92

E) 3.84

9) A 13.8 mL aliquot of 0.176 M H3PO4(aq) is to be titrated with 0.110 M NaOH (aq). What
volume (mL) of base will it take to reach the equivalence point?

A) 7.29

B) 22.1

C) 199

D) 66.2

E) 20.9

10) A solution is prepared by adding 1.60 g of solid NaCl to 50.0 mL of 0.100 M CaCl2. What is
the molarity of chloride ion in the final solution? Assume that the volume of the final solution is
50.0 mL.

A) 0.747

B) 0.647

C) 0.132
D) 0.232

E) 0.547

Report 2: Stoichiometry
(Total 80 points)

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code). This is only an advisory template of what needs to be include in your
complete lab write-up.

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Part 1

Data Table

Table 2.1.

Mass Grams

empty 150-mL beaker

NaHCO 3 in beaker

Mass of NaHCO 3

Table 2.2.

Mass Grams

NaCl plus beaker first weighing

NaCl plus beaker second weighing

NaCl plus beaker third weighing

1) The grams of NaHCO3 you had in your beaker was ________

2) Calculate how many moles of NaHCO3 the mass is ________

3) Write the molar ratio for the NaHCO3 / NaCl ratio _______

4) Write the number of moles of NaCl you predict were produced in your experiment.

5) Calculate the mass of NaCl you predict will be produced.

6) Determine, by subtraction, the actual mass of NaCl produced in your experiment.

a) first weighing

b) second weighing

c) third weighing

7) Calculate your percentage yield.

Discussion Questions

1. Compare the numerical value of the observed ratio for maximum yield to the best ratio

Part 2

Record your TAs value of the molarity of your solution.

Calculate your percent error from your assigned value.

Complete the equation for the titration of

NaHCO 3 aq + HCl aq →

Solutions
 Chapter 3. VSEPR: Molecular Shapes and Isomerism

Molecular Shapes & Isomerism

Objectives

Understand the 3-dimensional nature of molecules

Learn about Molecular Symmetry

Be able to identify the various isomers possible for one molecular formula

Be able to identify enantiomers

Grading
Quiz (10%).

Lab Report Form (90%).

Before Coming to Lab . . .

Look over the following to make sure you have a basic understanding of the topics presented.

Drawing Lewis Structures

Determining the Shapes of Molecules from their Lewis Structures

Some Basic Aspects of Bonding

Model Kits

Introduction

The shape of a molecule is extremely important in determining its physical properties and
reactivity. A multitude of shapes are possible, and in today’s lab, you will be looking at several.

In Part 1, you will be exploring the various symmetry elements that can be present in molecules.
The symmetry elements you will be looking for are mirror planes, rotation axes, and inversion
centers. Being able to determine which symmetry elements are present in a molecule help in
understanding its chemistry. If there is a plane present in the molecule that has the exact same
arrangement of atoms on either side of the plane, then the molecule has a mirror plane (σ). It is
important to note that a molecule can have more than one mirror plane. Rotation axes are
represented as Cn (n = 1, 2, 3 . . .). The subscript indicates how many degrees of rotation (360o/n)
are needed in order to return to the same orientation of atoms with which you started. So if there is
a C2 axis, the rotation would be 180o. An example of a molecule having a C2 axis is H2O.

Figure 3.1.

The third symmetry element is an inversion center (i). In such molecules, starting at any position
and drawing a line through the center and an equal distance to the opposite side of the molecule,
you will end up at a position with an identical environment to the one you started from.

Figure 3.2.

Part 2 of the lab introduces the concept of enantiomers. Enantiomers are molecules sharing the
same molecular configuration, but they are non-superimposable images of each other. This
concept should become clearer as you build the models for this part of the lab. Enantiomers share
many of the same physical properties. The property which distinguishes them is the direction in
which they rotate plane-polarized light. They will rotate the light in equal amounts but in different
directions (plane-polarized light is just light in which all wave vibrations have been filtered out
except for those in one plane). If both enantiomers are present in a 1:1 ratio, the effects of the
rotation of light cancel and no net rotation is observed. Such a mixture of isomers is known as a
racemic mixture or as a racemate. Because these isomers rotate plane-polarized light, they are
also known as optical isomers. Compounds that form optical isomers are said to be chiral.

The chemistry of enantiomers is of great importance in the field of medicine. It has been
discovered that with many drugs, one enantiomer will be biologically active while the other will
be inactive or even produce undesired side effects. For this reason, it has become advantageous for
pharmaceutical companies to try to synthesize the active enantiomer exclusively.

The next part of the lab deals with isomers. Isomers are molecules having the same molecular
formula, but the atoms are arranged in a different manner, while still obeying the rules of bonding.
There are different classifications for isomers. For example, structural isomers differ from one
another in the order in which the atoms are bound to each other (connectivity is different). On the
other hand, geometrical isomers have the same order of atoms, but the spatial arrangement of
atoms is different (connectivity is the same). A common example of geometrical isomers is the
cis and trans forms of double bonds:

Figure 3.3.

** NOTE: Remember that molecules having single carbon-carbon bonds cannot have cis/trans
isomers because there is free rotation about single bonds.

By building the models of various molecules during this lab, you will be able to better understand
molecular symmetry and isomers. Building models is not difficult; however, the chemical
principles involved are very important and you may find some surprises in how atoms can be fit
together.

Finally, in Part 4, you will be applying your knowledge of VSEPR (Valence Shell Electron Pair
Repulsion) Theory in order to determine the geometry of several different molecules. VSEPR
theory is useful in helping to determine how atoms will orient themselves in molecules. Basically,
the idea is that the arrangement adopted by a molecule will be the one in which the repulsions
among the various electron domains are minimized. The two kinds of electron domains are
bonding (electron pair shared by two atoms) and non-bonding (electron density centralized on one
atom) pairs of electrons.

Experimental Procedure

For Parts 1 & 2: You and your lab partner are to work with one other lab group in preparing these
models (no more than 3 - 4 students). Your TA will assign each group a certain set of molecules to
make and answer questions pertaining to those molecules. Each group will then present their
answers to the class. These models will need to be completed and answers determined within 30
minutes so that we can continue to Parts 3 & 4 as soon as possible.

For Parts 1-4, the work should be divided among the group members. Be sure to discuss the
questions and answers among yourselves, but put your own conclusions on the Report Form.
1. Symmetry Elements

Using the Molecular Framework models, make models of the following compounds:

1. CH4

2. CH3Cl

3. CH2Cl2

4. CHCl3

5. CH2ClF

6. CHBrClF

7. BF3

8. BF2Cl

9. PH3

10. PH2Cl

Choose a color to represent each atom. For example, make all C atoms black, all H atoms white,
etc.

Once the models are created, look for symmetry elements that may be present. Ask yourselves
the following questions:

Does the molecule contain a mirror plane (σ)? In other words, is there a plane within the
molecule which results in one half being a mirror image of the other half?

Does the molecule contain a two-fold rotation axis (C2)? Remember from the Introduction
that the subscript indicates the degrees of rotation necessary to reach a configuration that is
indistinguishable from the original one. In this case, the rotation will be 180o.

Does the molecule contain any higher-order rotation axes?

C3 – rotation by 120o

C4 – rotation by 90o

C∞ (infinity rotation axis) – rotation of any amount will result in an indistinguishable

 orientation

Does the molecule have an inversion center (i)?

Determine which of these symmetry elements are present in your assigned molecules. All of the
columns of the table on the report form should be filled out. If you have any difficulty
determining whether such symmetry elements are present in the molecules you are assigned, your
TA can provide examples of each symmetry element.

Extra credit points can be earned by indicating in the table how many of each symmetry element
are present for each molecule (i.e. How many mirror planes are present?).

2.Mirror Images

Using the model kits, build models which are the mirror images of the models you were assigned
to build (b, c, d, e, f, g, h, i and j) in Part 1. With the two mirror images in hand, try to place the
models on top of one another, atom for atom.

If you can do this, the model and its mirror image are superimposable mirror images of one
another. If not, the molecule and its mirror image form nonsuperimposable mirror images.
Nonsuperimposable mirror images are also known as enantiomers.

For each compound, decide whether the mirror image is superimposable or nonsuperimposable.
Can you make a generalization about when to expect molecules to have nonsuperimposable mirror
images?

3.Isomers

In this exercise you will build models of compounds which are structural and/or geometrical
isomers of one another.

Make the following models:

A. Structural Isomers

1. Make a model(s) of C2H5Cl. How many different structural isomers are possible?

2. Make a model(s) of C3H7Cl. How many different structural isomers are possible?

3. Make a model(s) of C3H6Cl2. How many different structural isomers are possible?

B. Geometrical Isomers

1. Make a model(s) of C2H3Cl. How many different structural and geometrical isomers are
possible?
2. Make a model(s) of C2H2Cl2. How many different structural and geometrical isomers are
possible?

3. Make a model(s) of cyclobutane (C4H8). HINT: cyclo = ring of C atoms

4. Now make dichlorocyclobutane (C4H6Cl2) by replacing two H atoms on cyclopropane with Cl

atoms. How many different structural and geometrical isomers are possible for
dichlorocyclobutane? You may wish to make a couple of cyclobutane molecules so that you
can compare the structures. Do any of the isomers have nonsuperimposable mirror images?

C. Aromatic Ring Compounds

1. Make a model of benzene, C6H6. Even though your model will contain alternating double and
single bonds, remember that in the real molecules of benzene all the C-C bonds are equivalent.
What symmetry elements does benzene possess?

2. Make a model(s) of chlorobenzene, C6H5Cl. How many different structural and geometrical
isomers are possible?

3. Make a model(s) of dichlorobenzene, C6H4Cl2. How many different structural and geometrical
isomers are possible?

4. Make a model(s) of trichlorobenzene, C6H3Cl3. How many different structural and geometrical
isomers are possible?

4. Hypervalent Structures

Hypervalent compounds are those that have more than an octet of electrons around them. Such
compounds are formed commonly with the heavier main group elements such as Si, Ge, Sn, Pb, P,
As, Sb, Bi, S, Se, Te, etc. but rarely with C, N or O. Refer to the rules for Electron Domain theory
in order to assign Lewis structures to the following molecules. Describe possible isomeric forms
and the bond angles between the atoms. How many lone pairs of electrons are present on the
central atom of each molecule, if any? (** Your book will be very useful in aiding you with these
structures **)

1. PF5

2. PF3Cl2

3. SF4

4. XeF2
5. BrF3

Solutions
 Chapter 4. Beer's Law and Data Analysis

Beer’s Law and Data Analysis

Objectives

Learn or review typical data analysis procedures – plotting data with excel, performing linear
regression analysis, etc.

Explore the concepts and applications of spectrophotometry

Grading

Pre-lab (10%)

Lab Report Form – including plot (80%)

TA points + Pop Quiz (10%)

Before coming to lab…

Read the lab instructions

Print out the lab instructions and report form.

Complete the pre-lab, due at the beginning of the lab

Introduction

When describing chemical compounds, scientists rely on their chemical and physical properties.
In lab, we might observe that a metal reacts violently with water, that a reactant is liquid at room
temperature, or that a powder is yellow. Chemical and physical properties can be used
qualitatively to identify a material or to predict its behavior, or quantitatively to determine how
much of that material is present in a solution. In this lab, we will develop a scheme to determine
the concentration of copper sulfate in aqueous solution using spectrophotometry.

To start, we will consider light and its interaction with matter. Chemicals exhibit a diverse range
of colors, especially when they contain transition metal ions. In order for a compound to have
color, it must absorb visible light. Visible light consists of electromagnetic radiation with
wavelengths ranging from approximately 400 nm to 700 nm, a small section of the
electromagnetic radiation spectrum shown below.

Light is characterized by its frequency ( ν), the number of times the crest of the wave passes some
point in space per second, or by its wavelength ( λ), the distance between two successive crests.
These two quantities are related by the speed of light, a fundamental constant: λν=c=3×108m/s.
Planck related the frequency of light to its energy (E) according to E=hν, where h is Planck's
constant, h=6.626×10−34J/s.

A compound will absorb light when the radiation posesses the energy needed to move an electron
from its lowest energy (ground) state to some excited state. The particular energies of radiation
that a substance absorbs dictate the colors that it exhibits. Conversely the color of a compound can
help us to determine its electronic configuration.

White light contains all wavelengths in this visible region. When a transparent sample (like most
aqueous solutions) absorbs visible light, the color we perceive is the sum of the remaining colors
that are transmitted by the object and strike our eyes.
 If an object absorbs all
wavelengths of visible light, none reaches our eyes, and it appears black. If it absorbs no visible
light, it will look white or colorless. If it absorbs all but orange, the material will appear orange.
We also perceive an orange color when visible light of all colors except blue strikes our eyes.
Orange and blue are complementary colors; the removal of blue from white light makes the light
look orange, and vice versa. Thus, an object has a particular color for one of two reasons: It
transmits light of only that color or it absorbs light of the complementary color.

Figure 4.1.

Complementary colors can be determined using an artist's color wheel. The wheel shows the
colors of the visible spectrum, from red to violet. Complementary colors, such as orange and blue,
appear as wedges opposite each other on the wheel.
With our eye, we can make qualitative judgments about the color(s) of light a sample absorbs.
However, given a red solution of [Ti(H2O)6]3+ we can not determine if it absorbs green light or if
it absorbs all colors of light but red. To quantitatively determine the amount of light absorbed by a
sample as a function of wavelength, we will measure its absorption spectrum using a UV-visible
spectrophotometer. Typical absorption spectra of aqueous [Ti(H2O)6]3+ solutions are shown
below.

Notice the absorption

maximum is at 490 nm. Because the sample absorbs more strongly in the green and yellow
regions of the visible spectrum, it appears red-violet. Measuring the absorption spectrum of a
second, more dilute solution demonstrates that the spectrum changes as a function of the
concentration of the solution. To understand how to use the absorption spectrum as a quantitative
tool for chemical analysis, read on!

Spectrophotmetric Basics

The essential components of a spectrophotometer consist of a radiation source, a wavelength

selector (monochromator), a photodetector and read-out device.
 Figure 4.2.

The incident light from a tungsten (visible light source) or deuterium (UV light source) lamp is
focused by a lens and passes through an entrance slit. By passing the beam through the
monochromator (either a prism or a diffraction grating) it is separated into monochromatic (i.e.,
one-color or single-wavelength) light. One particular wavelength of monochromatic light is
selected and allowed to pass through the exit slit into the sample. Light transmitted through the
sample is detected by a photodetector which converts the signal to an electrical current which is
measured by a galvanometer and sent to a recording device, typically a computer.

The measurement of transmittance (T) is made by determining the ratio of the intensity of
incident ( I0) and transmitted (I) light passing through pure solvent and sample solutions as a
function of wavelength. [Note: The percent transmittance (%T) is obtained by multiplication of T
by 100.] The logarithm of the reciprocal of the transmittance is called the absorbance (A),

A = log (1 / T)

Care must be taken when small values of transmittance are being measured as stray light from
either the room or scattering within the instrument can cause large errors in your readings!

Extracting Quantitative Information

The Beer-Lambert law relates the amount of light being absorbed to the concentration of the
substance absorbing the light and the pathlength through which the light passes:

A = εbc .

In this equation, the measured absorbance (A) is related to the molar absorptivity constant ( ε), the
path length (b), and the molar concentration (c) of the absorbing. The concentration is directly
proportional to absorbance.

The single largest application of the spectrophotometer is for quantitative analysis. The
prerequisite for such analysis is a known absorption spectrum of the compound under
investigation. Of particular importance is the maximum absorption (at λmax) [Why choose the
maximum? Could the choice alter the precision of our experiment? the accuracy?], which can be
easily obtained by plotting absorbance vs. wavelength at a fixed concentration. Next, a series of
solutions of known concentration are prepared and their absorbance is measured at λmax. Plotting
absorbance vs. concentration, a calibration curve can be determined and fit using linear regression
(least-squares fit). An unknown concentration can be deduced by measuring absorbance at the
absorption maximum and comparing it to the standard curve. Caution: The Beer-Lambert Law is
only obeyed (the standard curve is linear) for reasonably dilute solutions. Only those points in the
linear range of the standard curve may be used for accurate concentration determination.

Typical results are shown for the absorbance of [Ti(H2O)6]3+ measured at 490 nm.

Table 4.1.

Concentration (mg/mL) %Transmittance Absorbance

0 100. 0

1 50.0 0.301

2 25.0 0.602

3 12.5 0.903

Figure 4.3.

Over the studied range the solutions obey Beer's Law. If a solution has a measured absorbance of
0.450, we can calculate its concentration to be 1.5 mg/mL.

Experimental Procedure
In this experiment, each lab pair will measure the absorbance of CuSO4 at six concentrations. You
will create a calibration curve to correlate copper sulfate concentration to absorbance. This curve
will be used next week to determine the concentration of an unknown copper sulfate solution and,
in turn, the percent yield of a series of chemical reactions.

Materials CuSO4⋅5H2O distilled water pipette bulb 1cm cuvette 4 - 25 mL volumetric flask for
your dilutions

Note: You will be borrowing these and must collect them from your TA. Do not forget to return
the flask at the end of the lab). All students will lose 3 points in that lab section if any go missing!

100 mL volumetric flask for the parent solution (in your drawer)10 mL volumetric pipette or 10
mL graduated cylinder

1. Measure out an appropriate mass of CuSO4⋅5H2O to get 100ml of ~0.1M solution and record
the mass on your report form. Show your calculation to the TA before making the solution.
This is your parent solution. Calculate the molarity using the actual mass measured and record
it.

2. Do the following dilutions and calculate the concentrations for each.

Table 4.2.

Dilution (ml parent : ml total)

0:25 (DI H2O)

5:25

10:25

15:25

20:25

25:25 (parent solution)

1. Measure the absorbance of the 6 solutions you have prepared and the unknown given to you by
your TA.

Analysis

Plot the concentration as a function of absorbance for your six solutions. Perform a linear
regression analysis and determine the equation of a best-fit line.

PreLab: Spectrophotometry and Data Analysis – Beer’s Law

Hopefully here for the Pre-Lab

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

In many of the experiments that you will do throughout the duration of this course you will be
asked to analyze your data by making plots and calculating the best fit line through your data. One
program commonly used to analyze data in this fashion is Microsoft Excel ®. The following
exercise will help you through the process used to obtain a plot and linear regression for a set of
data.

Suppose you go for a 5 mile run and you tabulate the after each mile as in the following table.

Table 4.3.

Distance Traveled (miles) Time (sec)

1 510

2 1026

3 1548

4 2077

5 2612

Questions:

1. Plot the distance traveled in miles vs. the time in seconds.

2. Use linear regression to obtain a trendline and give the equation obtained in terms of the
variables distance traveled and time and the R-squared value. Comment on the meaning of the
R-squared value and its significance when doing data analysis.

3. Using the equation you obtained by doing linear regression, estimate how long the 6th mile
will take you to run.

4. Assuming this linear trend persists, how far have you run if you finish in 2900 sec.

EXCEL INSTRUCTIONS:
 In order to plot this data in excel, you should enter the data exactly as above in to column A
(rows 1-6) and column B (rows 1-6).

To plot the data you will need to go to Insert on the tool bar and then click Chart. A Chart
Wizard will appear. Select XY(Scatter) as the Chart type and choose the sub-type that does not
have any lines connecting the points, then click next.

On Step 2, click on the series tab near the top of the screen and click Add.

You do not need to name the series unless you have multiple plots on one graph, but you can
type in a name if you wish.

To insert the X data, click on the icon at the far left of the x series box.

Select the x values by clicking on the first one and while the left mouse button is down
dragging the mouse down to the last value.

When the values have been selected click the icon again and repeat for the y values. You may
also manually enter the values by separating them with a comma. Don’t forget you need to
remember what units you are using when answering questions.

Click next when you have x and y values entered correctly.

The next step is just entering title information and changing the appearance of your plot; click
next when finished.

Choose your chart location and then finish. You now need to place a linear regression line on
your plot.

Right click on a data point and pick add trendline.

Choose linear as the type and click the options tab.

Check the boxes to get the equation and R-squared value and click ok.

Solutions
 Chapter 5. Hydrogen and Fuel Cells

Hydrogen and Fuel Cells Experiment

Objective

Build a fuel cell in order to appreciate practically a range of important chemical and physical
principles, such as galvanic cells, energy conversion, energy quality, combustion reactions,
water electrolysis and bio-fuels.

Crituique the design in order to improve the efficiency of the fuel cell and to accomplish it
practically

Grading

Pre-lab (10%)

Lab Report (80%)

TA points (10%)

Before Coming to Lab…

Read the lab instructions

Introduction

As the world’s reserves of fossil fuels are diminishing and our awareness of environmental
protection is increasing, we strive to develop alternative ways of energy production. Thus in many
countries research into construction of stable and efficient fuel cells has been given high priority.
Indeed, President Bush in his January 28th 2003 State of the Union address, proposed a $1.2
billion fuel-cell research and development program.

Fuel cells are used for direction conversion of the energy of combustion reactions to electrical
energy. A possible fuel is hydrogen, which can be produced from water in electrolysis plants
driven by solar cells or windmills. A future interesting fuel source for operation fuel cells might
be “bio-fuels” i.e fuels produced from non-fossil organic material such as methane from biogas
plants, alcohol produced by fermentation of sugar or hydrolyzed starch (or, in the not so distant
future, perhaps also from enzymatically hydrolyzed cellulose).
Conventional power plants turn approximately 40% of the fuel energy into electricity; we say that
the efficiency of the plant is 40%. (Although, in some modern plants surplus heat is reused for
district heating thus increasing the actually efficiency somewhat). However, with fuel cells the
efficiency of chemical-to-electric energy conversion is unsurpassed, namely about 70% (or even
high in some experimental plants).

U.S. energy dependence is higher today than it was during the “oil shock” of the 1970’s, and oil
imports are project to increase. Passenger vehicles alone consume 6 million barrels of oil every
day, equivalent 85% of oil imports.

If just 20% of cars used fuel cells, we could cut oil imports by 1.5 million barrels a day.

If every new vehicle sold in the U.S. next year was equipped with a 60kW fuel cell, we would
double the amount of the country’s available electricity supply.

10,000 fuel cell vehicles running on non-petroleum feul would reduce oil consumption by 6.98
million gallons per year.

Fuel cells could dramatically reduce urban air pollution, decrease oil imports, reduce the trade
deficit and produce American jobs. The U.S. Department of Energy projects that if a mere 10% of
automobiles nationwide were powered by fuel cells, regulated air pollutants would be cut by one
million tons per year and 60 million tons of the greenhouse gas carbon dioxide would be
eliminated. DOE projects that the same number of feel cell cars would cut oil imports by 800,000
barrels a day – about 13% of total imports. Since fuel cells run on hydrogen derived from a
renewable source, the fuel cell emissions will be nothing but water vapor.

The Chemistry of a Fuel Cell

A fuel cell is a galvanic cell in which electricity is generated by a combustion reaction. The fuel
cell consists of two electrodes between which electrical contact is established by means of an
electrolyte. Oxygen or just plain atmospheric air is fed continuously to the cathode and the fuel is
fed continuously to the anode.

The fuel could be any of a vast number of combustible materials, e.g. methane, ethane or ethanol
(all organic fuels) hydrogen, hydrazine or sodium borohydride (inorganic fuels). With the
hydrogen burning cell as an example we can describe the chemistry of the cell by the following
reactions:

Anode – at which oxidation of the fuel takes place:

H2 + 2OH- -> 2H2O + 2e-

Cathode – at which reduction of oxygen takes places

½ O2 + H2O + 2e- -> 2OH-

The next reaction for the cell:

H2 + ½ O2 -> H2O

With ethanol as the fuel the matter becomes somewhat more complicated, since ethanol is
oxidized in steps to ethanal, ethanoic acid and carbon dioxide respectively. In an ideally working
fuel cell we assume that ethanal and ethanoic acid are further oxidized so that the only carbon
compound of the overall process is carbon dioxide. We have not succeed ( by simple chemical
tests) to detect either ethanol or ethanoic acid (or rather ethanoate due to the strongly basic
electrolyte solution) as intermediate products in our own cells. However we still suggest a three-
step oxidation of ethanol(and at the same time admitting that the last step is dubious):

Anode:

Step 1: CH3CH2OH + 2 OH- -> CH3CHO + 2 H2O + 2e-

Step 2: CH3HO + 2 OH- -> CH3COOH + H2O + 2 e-

Step 3: CH3COOH +8 OH- -> 2 CO2 + 6 H2O + 8 e-

Sum: CH3CH2OH + 12OH- -> 2 CO2 + 9 H2O + 12 e-

Cathode:

3O2 + 6 H2O + 12 e- -> 12OH-

Overall reaction:

CH3CH2OH + 3O2 -> 2CO2 + 3H2O

Sodium borohydride can power a cell in either a direct or indirect manner. Indirectly sodium
boroydride will decompose in water to produce NaBO2 (borax) and hydrogen

NaBH4 + 2H2O -> NaBO2 + 4H2

This hydrogen will then fuel the cell as shown above. However, sodium borohydride can directly
power a cell with higher energy yields.

Anode:

NaBH4 + 8OH- -> NaBO2 + 6H2O + 8e-

Cathode:
2O2 + 4H2O + 8e- -> 8OH-

While sodium borohydride costs ~$50 per kilogram, it has projected that mass production and
borax recycling could reduce that price to as low as $1 per kilogram.

Experimental

Caution!!! Plastic can burn.

To get good results, very careful measurements are required. Be sure to wear suitable eye
protection.

Materials:

2X 50-60mL disposable hypodermic syringes without needles and pistons.

3X pieces of nickel net (2 cut to cover the flanges of the syringe cylinders approximately 2cm
X 10cm + 1 extra piece) The net should be a very fine mesh.

2X machine screws with nuts and waters (all brass)

2X 20cm pieces of insulated 1mm copper wire with ~1.5cm insulation removed from each end

Heating plate

Aluminum plate 4-6mm thick with 7-8mm hole drilled through center

Baking paper

Screwdriver, drill, spanner, flat bit, scissors, wooden board and small saw

tape

Lab stand with clamps

600mL beakers

1.5V electric motor

Red LED

digital mulitimeter

balloons
 electrical leads with alligator clips

1M sodium hydroxide solution

4M nitric acid

ethanol

methanol

Palladium chloride solution (very expensive and should be recycled)

NaBH4

Oxygen gas

Hydrogen gas

Building an electrode (each group should build 2)

Cut a piece of nickel mesh to cover the flange of the syringe cylinder completely

Place an aluminum plate on a heating plate. Place the baking paper on the Al plate and the
nickel net on the paper.

Heat the plate to a temperature that will melt the plastic but not burn it.

4. Place the flange of the syringe on the nickel net on the heating plate. Press down firmly so
that the nickel net is melted onto the flange. Make sure that the net is sealed tight to the whole
of the flange surface, but take care not to melt so much plastic that the cylinder hold itself is
covered with molten plastic.

Remove the syringe and net form the eating plate and allow to cool.

At one of the sides of the flange drill a hole through the flange using the electric drill. Place a
piece of wood beneath to prevent drilling into the lab bench. (see picture) Push the machine
screw through the hole and fasten using a washer and nut. (see picture)

Mount a piece of insulated copper wire around the machine screw by twisting an end into a loop
with a flat bit and fastening it with the nut. Tighten it so that good electrical contact is
established between the wire and the nickel net. Use tape to attach the wire to the syringe
cylinder.

Cut off excess nickel net around the flange.

Clean the nickel net by immersing the electrode in 4M nitric acid for at least five minutes. Also
 Clean the nickel net by immersing the electrode in 4M nitric acid for at least five minutes. Also
clean the extra piece of nickel net in this manner. This much be carried out in the fume hood
since poisonous flumes may evolve. Rinse thoroughly with water.

Place the nickel net of the electrode in a solution of palladium chloride for 30 minutes and then
gently rinse with water. Be sure to put the extra piece of nickel net in the palladium chloride
solution as well. The electrode is now ready. You should have something that resembles the
picture.

Figure 5.1.

Figure 1: Drilling holes in flange.

Figure 5.2.

Figure 2: Wire connection assembly.

 Figure 5.3.

Figure 3: Final assembled cell

Building the cell

First cut top off of one of the syringes. This will be the electrode you introduce the liquid/solid
fuel.

Place your two electrodes into a 600mL beaker containing 1M NaOH solution. The nickel
meshing should be completely submerged in solution.

Fill a balloon with oxygen gas (from gas cylinder) and connect using rubber hosing to the
syringe that was not cut. The oxygen may bubble slowly through the syringe.

Roll up the extra piece of nickel mesh and place into the cut syringe.

Add ~20mg of NaBH4 to the syringe with the extra piece of nickel mesh. If time permits you
may test other fuels later.
 Figure 5.4.

Figure 4: Functional cell layout.

Testing the cell

Measure the voltage generated by your cell by taking a digital multimeter and setting it to DC
voltage. Connect one probe to each wire of the cell. The reading may continue to grow for a
while and then stabilize. Record this stable voltage. It should read between 0.8V-1V.

Measure the current your cell sources by keeping the probes connected and switching to current
mode. This reading should be between 30mA-50mA.

Powering an LED

One fuel cell does not generate enough voltage to power anything of interest. Just like you
would connect 2 or 4 AA batteries in series to power a portable CD player, it is necessary to
connect multiple fuel cells to generate larger voltages.

Pair up with another group and connect the positive terminal of one cell to the negative
terminal of the other cell using the wires with alligator clips. Now connect the unwired positive
terminal to the positive (longer lead) of the red LED. The unwired negative terminal should be
connected to the negative (short lead) of the red LED. At this point the LED should be lit. If
you do not see any light, you should use the multimeter to check the voltage generated by the
two cells in series and verify that it is greater that 1.5V. If you do not measure any voltage
verify that you have wired everything correctly.
 Figure 5.5.

Figure 5.6.

Figure 5: Powering an LED circuit.

Powering a small motor

While two cells in series generate the proper voltage to operate the motor, they cannot source
enough current to run a motor longer than a few seconds. By putting cells in parallel more
current can be obtained.

You will need two sets of two cells in series as described in the “Powering an LED” section (4
groups are needed for this part).

Take the positive connection from each series cell and connect to one terminal of the electric
motor. Take the negative connection from each series cell and connect to the other terminal on
the electric motor. At this point the motor shaft should begin to turn. If not, check the wiring
and verify that you are applying at least 1.5V. It is also possible that 2 parallel cells will not
generate enough current. Additional cells can be added in parallel to generate more current.
 Figure 5.7.

Figure 6: Powering a motor circuit.

Pre-Lab: (Total 10 Points)

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

1.Fill in the blanks:

Fuel cells are used for direction conversion of the energy of combustion reactions to
______________. A fuel cell is a ______________ in which electricity is generated by a
combustion reaction. A fuel cell provides a ______________ voltage that can be used to power
motors, lights or any number of electrical appliances.

2.T or F At the anode, oxidation of the fuel takes place.

3.T or F The fuel cell emissions will be nothing but water vapor.

4.T or F The efficiency of fuel cells, chemical-to-electric energy conversion, is approximately

40%.

Review of series and parallel circuits:

In a series circuit, the electrons in the current have to pass through all the components, which are
arranged in a line. Consider a typical series circuit in which there are three resistors of value R1,
R2, and R3.
 Figure 5.8.

There are two key points about a series circuit:

The current throughout the circuit is the same.

The voltages add up to the battery voltage.

Therefore:

VT = V1 + V2 + V3

From Ohm’s Law:

VT = IRT;

V1 = IR1;

V2 = IR2;

V3 = IR3

Þ IRT = IR1 + IR2 + IR3

Therefore:

RTot = R1 + R2 + R3

5.In the circuit below, the current is 100 mA.

 Figure 5.9.

(a) What is the current in each resistor?

(b) What is the voltage across each resistor?

(c) What is the total resistance?

(d) What is the battery voltage?

Figure 5.10.

Parallel circuits have their components in parallel branches so that an individual electron can go
through one of the branches but not the others. The current splits into the available number of
branches.

In this case, the current will split into three. For a parallel circuit:

The voltage across each branch is the same.

The currents in each branch add up to the total current.

From this:

Itot = I1 + I2 + I3

From Ohm’s Law: I T = V ; I1 = V; I2 = V; I3 = V

RT R1 R2 R3

ÞV=V+V+V

RT R1 R2 R3

Þ 1/RTot = 1/R​1 + 1/R2 + 1/R3

6.This question refers to the circuit below.

Figure 5.11.

(a) What is the total resistance of the circuit?

(b) What is the current through each resistor?

(c) What is the total current?

Figure 5.12.

For resistors in both series and parallel, follow these guidelines:

Work out the total resistance of the parallel combination.

Work out the total resistance of the circuit by adding your answer in the previous step to the
values of the series resistors.

7.What is the single resistor equivalent of this circuit?

 Report (80 points)

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

The following tables and questions should be answered in your written report. Please put the
information in the relevant section of your report (i.e. observations and results, discussion)

What would happen if zinc screws were used instead of brass?

What is the purpose of the palladium coating on the anode?

What is the purpose of the palladium coating on the cathode?

What fuel cell worked best?

Explain, in detail, why you think that the best fuel cell worked better than the others?

Debate fuel cells.

Solutions
 Chapter 6. The Best Table in the World

The Best Table in the World!

Objective

The goals of this experiment are:

to observe the reactions of several metals with cold water, hot water, acids and then other metal
ions.

to prepare an activity series of the metals based on the observations from the above reactions.

Grading

You will be assessed on:

observations of the reactions of several metals with cold water, hot water, acids and then other
metal ions.

preparation of an activity series of the metals based on the observations from the above
reactions.

answers to the post-lab questions.

Background Information

First, you are going to travel back to 1869 and marvel at how the first periodic law and table were
born when only 63 elements had been discovered at the time. A 35 year old professor of general
chemistry, Dmitri Ivanovich Mendeleev at the University of St. Petersburg (now Lennigrad) in
Russia was shuffling his cards with the properties of each element on each card trying to organize
his thoughts for his soon-to-be famous textbook on chemistry. When he realized that if the
elements were arranged in the order of their atomic weights, there was a trend in properties that
repeated itself several times! His paper was delivered by his graduate student, Nikolai
Aleksandrivich Menchutkin before the Russian Chemical Society while Medeleev was busy
visiting cheesemaking cooperatives at the time!

In order to see and find order among the elements, we must have some general acquaintance with
them. Elements are made of matter, and matter is defined as anything that has mass and occupies
space. This includes everything that you can see and a lot that you cannot. It follows that in order
to distinguish between different types of matter (in other words different elements) we have to
assess their properties.

There are two types of properties: intensive and extensive. In the former case, intensive properties
do not depend on the how much of an element is present but do include state (whether a substance
is a solid, liquid or gas), color and chemical reactivity. Extensive properties depend on the
quantity of matter present - mass and volume are extensive properties.

Properties can be further categorized as either chemical or physical. A chemical change describes
how the substance may change composition, such as spontaneously by combustion or in
combination with other substances. On the other hand, physical changes are those properties that
can be measured without changing the composition of the matter. Condensation of steam to water
is a physical change.

Introduction

What is there to know about the periodic table? Why is it important? Why does it appear in nearly
every science lecture room and labs? Is it just a portrait of an aspect of chemistry or does it serve
a useful purpose? Why is the name periodic appropriate? Why is the table arranged in such a way?
What are the important features of the table? Does it give order to the approximately 120 known
elements?

Relative Reactivity of Metals and the Activity Series

A superficial glance at the Periodic Table will reveal that all known elements are listed by their
chemical symbols. An in depth glance at the Periodic Table yields information on the mass of an
atom of the element in atomic mass units (amu) for the molar mass of a mole ( 6.02×1023) of
atoms in grams below the chemical symbol for each element. Above the chemical symbol for each
element, there is a second number listed, the atomic number, which gives the number of protons
(positively charged particles in the nucleus), or the number of electrons (negatively charged
outside the nucleus) for a neutral atom.

Mendeleev arranged the elements in the Periodic Table in order of increasing atomic number in
horizontal rows of such length that elements with similar properties recur periodically; that is to
say, they fall directly beneath each other in the Table. The elements in a given vertical column are
referred to as a family or group. The physical and chemical properties of the elements in a given
family change gradually as one goes from one element in the column to the next. By observing the
trends in properties, the elements can be arranged in the order in which they appear in the Periodic
Table.

Procedure
 I. Activity Series

Part 1. Reactions of Metals with Water

CAUTION! Sodium reacts very rapidly with water to evolve hydrogen and heat. This is potentially
dangerous because of the possibility of the violent explosive reaction of H2 (g) with O2 (g) present
in the air.

CAUTION! Sodium causes severe chemical burns when it comes into contact with the skin. Note:
Metallic sodium must be stored below the surface of an inert liquid such as kerosene to prevent
oxidation by air.

1. I will demonstrate the reaction of sodium and then potassium with water. Observe the rate of
evolution of H2 gas as I use tweezers to place a tiny pea-size piece of sodium then potassium
into a 500-mL beaker full of deionised water. Record your observation on the Report Form and
write a balanced equation for this reaction.

2. Place 5 mL H2O in each of four clean tubes and label them as follows:

Table
6.1.

A. Mg

B. Cu

C. Zn

D. Ca

1. Use sandpaper or steel wool to remove the oxide from the surfaces of Mg, Cu, and Zn.

2. Place several small pieces of Mg, Cu, and Zn in the correctly labeled test tube prepared above.
Place two or three (not more!) pieces of Ca turnings in the test tube labeled "Ca".

3. Watch for evidence of reaction by noting evolution of gas bubbles and any change in the color
or size of the metal. Record your observations and write net ionic equations for each reaction.

Note: Trapped air bubbles on the metal surfaces are not indicative of a reaction.

CAUTION: H2 is FLAMMABLE!
CAUTION: Residual calcium should be discarded in a special container designated by your
instructor.

Note: Net ionic equations must balance in mass (atoms) and in total charge on each side of the
equation.

Part 2. Reactions of Metals with HCl

CAUTION: The reaction of Ca with HCl is not studied. Residual calcium should be discarded in a
special container designated by your instructor.

1. Decant the water from each test tube used in the procedure above and leave the pieces of metal
that remain unreacted in each test tube.

2. Place the test tubes in a test tube rack/holder.

3. Add 2 mL of 3 M HCl solution to each test tube.

CAUTION: Some of the test tubes may become very hot. Leave them in the rack/holder while you
are making observations.

1. Observe relative rate of H2 gas evolution for up to 10 minutes and record your observations on
your report form.

2. Based on the observations in the previous steps, list the elements that react in 3M HCl in order
of increasing strength as reducing agents and write net ionic equations for all reactions.

Part 3. Reactions of Metals with Other Metal Ions

1. Place a clean 1 inch-square of metal foil (sheet) of each of these metals Cu, Zn and Pb on a flat
surface.

2. Clean the metal surfaces by sanding them with fine sandpaper or steel wool.

3. Place one or two drops in spots of each of these solutions in a clockwise order on the metal
surfaces:

Table 6.2.

A. 0.5 M Ag+

B. 0.5 M Cu2+

C. 0.5 M Zn2+
 D. 0.5 M Pb2+

1. NOTE: Do not test a cation of a metal on a square of the same metal such as Cu2+ ion and Cu
metal.

2. Watch for color changes in each spot as evidence of reaction. If you are not sure whether the
reaction has occurred, rinse the plate with water. A distinct spot of a different color on the
surface is good evidence for the reaction.

3. Write net ionic equations for each reaction . Arrange Ag, Cu, Pb and Zn in order of their
increasing strength as reducing agents. If a metal A reacts with a cation of another metal B,
metal A is a stronger reducing agent, more reactive than metal B.

4. Rinse and dry each square of metal and return it to the correct beaker on the reagent shelf for
other students to use.

Part 4. Flame Tests

One station set up that all sections will rotate through

Clean a spatula wire by dipping it into dilute hydrochloric acid (3M) and then holding it in a hot
Bunsen flame. Repeat this until the spatula doesn't produce any color in the flame.

When the spatula is clean, moisten it again with some of the acid and then dip it into a small
amount of the solid you are testing so that some sticks to the spatula. Place the spatula back in the
flame again.

If the flame color is weak, it is often worthwhile to dip the spatula back in the acid again and put it
back into the flame as if you were cleaning it. You often get a very short but intense flash of color
by doing that.

Chemicals/Materials:

1. Chloride salts of Li, Na, K, Rb, Cs, Ca, Ba, Cu, Pb, Fe (II) and Fe(III) Sr (nitrate salt).

2. Glass rods with loops of Pt wire.

3. Bunsen burner/clicker.

4. Concentrated nitric acid or hydrochloric acid.

Record your observations on your report form.

It should be noted that sodium is present as an impurity in many if not most metal salts. Because
sodium imparts an especially intense color to a flame, flashes of the sodium may be observed in
nearly all solutions tested.

Pre-Lab 5: The Best Table in the World!

Hopefully here for the Pre-Lab

Name(Print then sign): __________________________________________________

Lab Day: ___________________Section: ________TA________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

1. The mass of an atom of the element in atomic mass units (amu) for the molar mass of a mole (
6.02×1023) of atoms in grams above or below the chemical symbol for each element? Circle
the correct one.

2. The second symbol listed for each element is the _______ __________, symbol ________?
Fill in the blanks.

3. The number in question 2 gives the number of

____________ or

the number of ________________ for a neutral atom. Fill in the blanks

4. The elements in a given vertical column are referred to as a _________ or __________. Fill in
the blanks.

5. The horizontal rows are called __________? Fill in the blank

6. The block of elements between groups II and III are called ___________ _________? Fill in
the blanks.

7. Elements 58 to 71 are known as ____________ or __________________? Fill in the blanks.

8. Elements 90 to 103 are known as _________ ____________? Fill in the blanks.

9. Do elements with larger atomic numbers than 92 occur naturally? True or false? Circle the
correct one.

Report 5: The Best Table in the World!

Hopefully here for the Report Form

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): __________________________________________________

Lab Day: ___________________Section: ________TA________________________

I. Activity Series

Part 1. Reactions of Metals with Water

Table 6.3.

Metal Observations Net Ionic Equations (If NoReaction Occurs, write N.R)

Na

Mg

Cu

Zn

Ca

Part 2. Reactions with HCl

Table 6.4.

Metal Observations Net Ionic Equations (If No Reaction Occurs, Write N.R.)

Mg

Cu

Zn
2. Based on your experimental results place Mg, Cu, Zn and Ca in order of increasing strength as
reducing agents.

Part 3. Reactions with Other Metal Ions

1. Write in the appropriate box either “REACTION” or “NO REACTION”.

Table 6.5.

Zn Cu Pb

Ag +

Cu 2 + Do not test

Zn 2 + Do not test

Pb 2 + Do not test

2. Write balanced equations to represent the results tabulated above.

3. Based on your experimental results, arrange Ag, Cu, Zn and Pb in order of increasing strength
as reducing agents.

4. Arrange Ag+, Cu2+, Zn2+ and Pb2+ in order of increasing strength as oxidizing agents.

5. Combine the results from Part 2 and Part 3. Arrange Mg, Cu, Zn, Ca, Ag and Pb in order or
increasing strength as reducing agents.

6. Place Ni in this row, if it is found that Ni will deposit on Zn foil, but not on Pb foil when a drop
of NiSO4 is placed on both.

Part 4. Flame Tests

Table 6.6.

Element Color in flame

Li

Na

K
 Rb

Cs

Ca

Sr

Ba

Cu

Pb

What are the limitations of this test?

Solutions
 Chapter 7. Bonding 07

Lab 5: Bonding 07

Objective
To test various compounds and determine their conductivity and bonding.

To understand how electronegativity can predict bond type.

To learn the relationship between bonding and conductivity.

Grading
Pre-Lab (10%)

Lab Report Form (80%)

TA Points (10%)

Background Information
A chemical bond is a link between atoms that results from the mutual attraction of their nuclei for
electrons. Bonding occurs in order to lower the total potential energy of each atom or ion.
Throughout nature, changes that decrease potential energy are favored.

The main types of bonds that we will be covering are ionic bonds, covalent bonds, and metallic
bonds. An ionic bond is the chemical bond that results from the electrostatic attraction between
positive (cations) and negative (anions) ions. The ionic relationship is a “give and take”
relationship. One ion donates or “gives” electrons, while the other ion receives or “takes”
electrons.

A covalent bond is a chemical bond resulting from the sharing of electrons between two atoms.
There are two main types of covalent bonds. The first being non-polar covalent bonds. These are
bonds in which the bonding electrons are shared equally by the united atoms-with a balanced
electrical charge. Polar covalent bonds are covalent bonds in which the united atoms have an
unequal attraction for the shared electrons.
 Figure 7.1.

The role of electrons in bonding has been well-studied. The ability of an atom or element to attract
electrons to itself is known as the element’s electronegativity. A scale was first calculated by the
Nobel laureate Linus Pauling and is commonly called the Pauling electronegativity scale. The
actual electronegativity values aren’t as important as how they compare to a different element. In
Part I of today’s experiment, you will compare electronegativity values to predict the type of bond
that will exist between two elements.

In the solution state, ionic compounds dissociate to give a separation of charge. The separation of
charge allows for the flow of electrons through solution. The flow of electrons is classified as
conductivity. A strong electrolyte is a compound that when dissolved in water will completely
ionize or dissociate into ions. That is, the compound exists in water only as individual ions, and
there are no intact molecules at all. This solution conducts electricity well. A weak electrolyte is
a compound that when dissolved in water only partially ionizes or dissociates into ions. That is,
the compound exists in water as a mixture of individual ions and intact molecules. This solution
conducts electricity weakly. A nonelectrolyte is a compound that when dissolved in water does not
ionize or dissociate into ions at all. In water, this compound exists entirely as intact molecules.
The solution does not conduct electricity at all. By measuring the conductivity of a dissolved
compound, we can classify it as a nonelectrolyte, weak electrolyte, or strong electrolyte and
determine its ability to dissociate into ions. There are four common compounds that you will
encounter in today’s lab.

ACIDS are molecular compounds which ionize (turn into ions) in water. The cation that is formed
is always H+. Therefore, in the formulas for simple acids, H is always the first element listed.
Some acids are strong electrolytes and some acids are weak electrolytes. There are no acids which
are nonelectrolytes because by definition an acid is a H+ donor.

BASES can be molecular compounds or ionic compounds. Some bases are soluble and some are
not. The soluble bases ionize or dissociate into ions in water, and the anion formed is always
OH−. The ionic bases have hydroxide ( OH− ) as the anion. If they are soluble, the ions simply
separate (dissociate) in the water. All of the ionic bases which are soluble are strong electrolytes.

SALTS are ionic compounds which are not acids or bases. In other words, the cation is not
hydrogen and the anion is not hydroxide. Some salts are soluble in water and some are not. All of
the salts which are soluble are relatively strong electrolytes.

NONELECTROLYTES are compounds which dissolve in water but do not ionize or dissociate into
ions. These would be molecular compounds other than the acids or bases already discussed.

Experimental Procedure
Caution:Acids and bases are corrosive and can cause burns.

Part I. Predicting bond type through electronegativity differences.

Using the electronegativity table provided in the lab manual, predict the type of bond that each of
the following compounds will have by the following process:

Find the electronegativity for each element or ion in compound using electronegativity table
provided.

Subtract the electronegativites (using absolute value).

If values are between:

4.0-1.7---Ionic bond-50-100% ionic

1.7-0.3---Polar Covalent bond-5-50% ionic

0.3-0.0---Non-Polar Covalent-0-5% ionic

Determine the type of bonding in the following compounds: KCl, CO, CaBr2, SiH4, MgS.
 Figure 7.2.

Part II. Weak and strong electrolytes

Chemicals

tap water

0.1 M hydrochloric acid, HCl

0.1 M acetic acid, HC2H3O2

0.1 M sulfuric acid, H2SO4

0.1 M sodium hydroxide, NaOH

0.1 M ammonia, NH3

0.1 M sodium acetate, NaC2H3O2

0.1 M sodium chloride, NaCl

 0.1 M ammonium acetate, NH4C2H3O2

0.1 M ammonium chloride, NH4Cl

methanol, CH3OH

ethanol, C2H5OH

sucrose solution, C12H22O11

In today’s lab, you will be using a MicroLab conductivity probe to determine how well electrons
flow through a given solution. First, you will need to calibrate the probe with a non-electrolyte
(distilled water) and a very strong electrolyte. To quantify how well a solution conducts, we will
assign numerical values to the conductance probe. A non-conducting solution will have a
conductance value of 0, a poor conducting solution will have a reading of 0 to 1,000, and good
conductors will have readings of 3,000 up.

Instructions for MicroLab Conductivity Experiment

Open the MicroLab Program by clicking on the Shortcut to MicroLab.exe tab on the desktop.

On the “Choose an Experiment Type” Tab, enter a name for the experiment, and then double click
on the MicroLab Experiment icon

Click “Add Sensor”, Choose sensor = Conductivity Probe

Choose an input, click on the red box that corresponds to the port that your conductivity sensor is
connected to. Choose 20,000 microseconds

“Choose a Sensor”, click radial button that says Conductivity Probe. Click next.

Click “Perform New Calibration”

Click “Add Calibration Point” place the conductivity probe in the non-conductive standard
solution, while swirling wait until the value is constant and then enter 0.0 into the “Actual Value”
box in MicroLab and hit “ok”.

Again, Click “Add Calibration Point” place the conductivity probe in the conducting standard
solution, while swirling wait until the value is constant and then enter 1020 into the “Actual
Value” box in MicroLab and hit “ok”. Repeat for 3860 as the Actual Value.

Under Curve Fit Choices , click on “First order (linear)” and then “Accept and Save this
Calibration”, when prompted to “Enter the units for this calibration”, leave as is and click ok, save
as your name-experiment-date. Click finish.

In the sensor area, left click on the conductivity icon and drag it to the Y-axis over “data source
two”, also click and drag to column B on the spreadsheet and also click and drag to the digital
display window.

When ready to obtain data, click start.

This is very important: Be sure to thoroughly since the probe with DI water between every use.

Beginning with the tap water, measure the conductance of each of the following solutions. Using
the information provided in the lab manual, classify each solution as a non-, weak, or strong
electrolyte. For those solutions that are electrolytes, record the ions present in solution.

Part III. Electrolyte strength and reaction rate

Chemicals

calcium carbonate powder - shake once

1 M HCl - stopper it

1 M HC2H3O2

0.5 M H2SO4

Test tube gas collection apparatus - end at 20mL

Measure 2 g of powdered calcium carbonate ( CaCO3) onto a piece of weigh paper. Obtain 30 mL
of 1 M HCl in a graduated cylinder. Pour the acid into the test tube apparatus. Add the calcium
carbonate to the acid and QUICKLY stopper the tube to begin collecting gas. Record the time it
takes to collect 20 mL of gas. The acid may react very fast with the CaCO3 generating the gas very
rapidly. Clean out the test tube apparatus and repeat the experiment using 1 M HC2H3O2 and 0.5
M H2SO4.

Part IV. Chemical reactions

Chemicals

0.01 M calcium hydroxide, Ca(OH)2

Plastic straws
Obtain ~20 mL of saturated calcium hydroxide solution. Make sure it is clear and colorless. Place
the conductivity probe in the solution and begin monitoring it conductivity. With your straw,
slowly exhale into the solution. Note any observations in the solution and the conductivity.

Pre-Lab 5: Bonding 07

(Total 10 Points)
Hopefully here for the Pre-Lab

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

Part I. Bonding of chemicals in solution

1. Write out the formulas of the following acids:

phosphoric ____________________

perchloric ____________________

nitric ____________________

sulfuric __________________

hydrochloric ____________________

acetic ____________________

1. Write out the formulas of the following bases:

calcium hydroxide ____________________

potassium hydroxide ____________________

sodium hydroxide ____________________

ammonia ____________________

1. Write out the formulas of the following salts:

 potassium chromate ____________________

potassium sulfate ____________________

copper(II) nitrate ____________________

calcium carbonate ____________________

potassium iodide ____________________

Report 5: Bonding 07
Hopefully here for the Report Form

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Part I. Predicting bond type through electronegativity differences.

Table 7.1.

Chemical Formula Electroneg (1) Electroneg (2) Diff Electroneg Type of bond

KCl

CO

CaBr 2

SiH 4

MgS

Part II. Weak and strong electrolytes

Table 7.2.

Solution Tested Numerical Output Electrolyte Strength Ions Present

 0.1 M HCl

0.1 M HC2H3O2

0.1 M H2SO4

0.1 M NaOH

0.1 M NH3

0.1 M NaC2H3O2

0.1 M NaCl

0.1 M NH4C2H3O2

0.1 M NH4Cl

CH 3 OH

C 2 H 5 OH

Sucrose

Tap water

1. Why do we use deionized water instead of tap water when making solutions for conductivity
measurements?

Part III. Electrolyte strength and reaction rate

2. Time to collect 20 mL of gas using 1 M HCl _______________________. Write the reaction of

HCl with CaCO3.

3. Time to collect 20 mL of gas using 1 M HC2H3O2_______________________. Write the

reaction of HC2H3O2 with CaCO3.

4. Time to collect 20 mL of gas using 0.5 M H2SO4_________________________.Write the

reaction of H2SO4 with CaCO3.

5. Why does it take different lengths of time to collect 20 mL of gas?

6. Based on the time it took to collect 20 mL of gas, rank the acids in the order of increasing
strength.
7. Why did we use 0.5 M H2SO4 instead of 1.0 M H2SO4?

Part IV. Chemical reactions

8. Write the chemical reaction for calcium hydroxide with your exhaled breath.

9. Write your observations for the reaction that took place (i.e. appearance, conductivity, etc.)

10. When in separate solutions, aqueous ammonia, NH3(aq) and acetic acid HC2H3O2 conduct
electricity equally well. However, when the two solutions are mixed a substantial increase in
electrical conductivity is observed. Explain.

11. Separately, ammonium sulfate and barium hydroxide solutions are very good conductors.
When the two solutions are mixed a substantial decrease in conductivity is observed. Rationalize
this.

Solutions
 Chapter 8. Solid State and Superconductors

Solid State Structures and Superconductors

Objectives

Build examples of: simple cubic, body centered cubic and face centered cubic cells.

Understand and familiarize with three-dimensionality of solid state structures.

Understand how binary ionic compounds (compounds made up of two different types of ions)
pack in a crystal lattice.

Observe the special electromagnetic characteristics of superconducting materials using 1,2,3-

superconductor , discovered in 1986 by Dr. Paul Chu at the University of Houston.

Grading

Your grade will be determined according to the following

Pre-lab (10%)

Lab report form. (80%)

TA points (10%)

Before coming to lab:

Read introduction and model kits section

Complete prelab exercise

Introduction

From the three states of matter, the solid state is the one in which matter is highly condensed. In
the solid state, when atoms, molecules or ions pack in a regular arrangement which can be
repeated "infinitely" in three dimensions, a crystal is formed. A crystalline solid, therefore,
possesses long-range order; its atoms, molecules, or ions occupy regular positions which repeat in
three dimensions. On the other hand an amorphous solid does not possess any long-range order.
Glass is an example of an amorphous solid. And even though amorphous solids have very
interesting properties in their own right that differ from those of crystalline materials, we will not
consider their structures in this laboratory exercise.

The simplest example of a crystal is table salt, or as we chemists know it, sodium chloride (NaCl).
A crystal of sodium chloride is composed of sodium cations ( ) and chlorine anions ( ) that
are arranged in a specific order and extend in three dimensions. The ions pack in a way that
maximizes space and provides the right coordination for each atom (ion). Crystals are three
dimensional, and in theory, the perfect crystal would be infinite. Therefore instead of having a
molecular formula, crystals have an empirical formula based on stoichiometry. Crystalline
structures are defined by a unit cell which is the smallest unit that contains the stoichiometry and
the “spatial arrangement” of the whole crystal. Therefore a unit cell can be seen as the building
block of a crystal.

The crystal lattice

In a crystal, the network of atoms, molecules, or ions is known as a crystal lattice or simply as a
lattice. In reality, no crystal extends infinitely in three dimensions and the structure (and also
properties) of the solid will vary at the surface (boundaries) of the crystal. However, the number
of atoms located at the surface of a crystal is very small compared to the number of atoms in the
interior of the crystal, and so, to a first approximation, we can ignore the variations at the surface
for much of our discussion of crystals. Any location in a crystal lattice is known as a lattice point.
Since the crystal lattice repeats in three dimensions, there will be an entire set of lattice points
which are identical. That means that if you were able to make yourself small enough and stand at
any such lattice point in the crystal lattice, you would not be able to tell which lattice point of the
set you were at – the environment of a lattice point is identical to each correspondent lattice point
throughout the crystal. Of course, you could move to a different site (a non-correspondent lattice
point) which would look different. This would constitute a different lattice point. For example,
when we examine the sodium chloride lattice later, you will notice that the environment of each
sodium ion is identical. If you were to stand at any sodium ion and look around, you would see the
same thing. If you stood at a chloride ion, you would see a different environment but that
environment would be the same at every chloride ion. Thus, the sodium ion locations form one set
of lattice points and the chloride ion locations form another set. However, lattice points not only
exist in atom positions. We could easily define a set of lattice points at the midpoints between the
sodium and chloride ions in the crystal lattice of sodium chloride.
The unit cell

Since the crystal lattice is made up of a regular arrangement which repeats in three dimensions,
we can save ourselves a great deal of work by considering the simple repeating unit rather than the
entire crystal lattice. The basic repeating unit is known as the unit cell. Crystalline solids often
have flat, well-defined faces that make definite angles with their neighbors and break cleanly
when struck. These faces lie along well-defined directions in the unit cell.

The unit cell is the smallest, most symmetrical repeating unit that, when translated in three
dimensions, will generate the entire crystal lattice.

It is possible to have a number of different choices for the unit cell. By convention, the unit cell
that reflects the highest symmetry of the lattice is the one that is chosen. A unit cell may be
thought of as being like a brick which is used to build a building (a crystal). Many bricks are
stacked together to create the entire structure. Because the unit cell must translate in three
dimensions, there are certain geometrical constraints placed upon its shape. The main criterion is
that the opposite faces of the unit cell must be parallel. Because of this restriction there are only
six parameters that we need to define in order to define the shape of the unit cell. These include
three edge lengths a, b, and c and three angles α, β and γ. Once these are defined all other
distances and angles in the unit cell are set. As a result of symmetry, some of these angles and
edge lengths may be the same. There are only seven different shapes for unit cells possible. These
are given in the chart below.

Table 8.1.

Highest Type of Symmetry Element

Unit Cell Type Restrictions on Unit Cell Parameters
Required

a is not equal to b is not equal to c; α is no symmetry is required, an

Triclinic
not equal to β is not equal to γ. inversioncenter may be present

a is not equal to b is not equal to c α = highest symmetry element allowed

Monoclinic
γ 90° β is not equal to 90°. is aC2 axis or a mirror plane

has three mutually

a is not equal to b is not equal to c α=
Orthorhombic perpendicularmirror planes and/or
β = γ 90°
C2 axes
Tetragonal a =b is not equal to c α = β = γ 90° has one C4 axis

Cubic a =b =c α = β = γ 90° has C3 and C4 axes

Hexagonal, a =b is not equal to c α = β = 90° C6 axis (hexagonal); C3 axis

Trigonal γ 120° (trigonal)

Rhombohedral* a =b =c α = β = γ is not equal to 90° C3 axis (trigonal)

*There is some discussion about whether the rhombohedral unit cell is a different group or is
really a subset of the trigonal/hexagonal types of unit cell.

Stoichiometry

You will be asked to count the number of atoms in each unit cell in order to determine the
stoichiometry (atom-to-atom ratio) or empirical formula of the compound. However, it is
important to remember that solid state structures are extended, that is, they extend out in all
directions such that the atoms that lie on the corners, faces, or edges of a unit cell will be shared
with other unit cells, and therefore will only contribute a fraction of that boundary atom. As you
build crystal lattices in these exercises you will note that eight unit cells come together at a
corner. Thus, an atom which lies exactly at the corner of a unit cell will be shared by eight unit
cells which means that only ⅛ of the atom contributes to the stoichiometry of any particular unit
cell. Likewise, if an atom is on an edge, only ¼ of the atom will be in a unit cell because four unit
cells share an edge. An atom on a face will only contribute ½ to each unit cell since the face is
shared between two unit cells.

It is very important to understand that the stoichiometry of the atoms within the unit cell must
reflect the composition of the bulk material.

Binding forces in a crystal

The forces which stabilize the crystal may be ionic (electrostatic) forces, covalent bonds, metallic
bonds, van der Waals forces, hydrogen bonds, or combination of these. The properties of the
crystal will change depending upon what types of bonding is involved in holding the atoms,
molecules, or ions in the lattice. The fundamental types of crystals based upon the types of forces
that hold them together are: metallic in which metal cations held together by a sea of electrons,
ionic in which cations and anions held together by predominantly electrostatic attractions, and
network in which atoms bonded together covalently throughout the solid (also known as covalent
crystal or covalent network).
Close-packing

Close-packing of spheres is one example of an arrangement of objects that forms an extended

structure. Extended close-packing of spheres results in 74% of the available space being occupied
by spheres (or atoms), with the remainder attributed to the empty space between the spheres. This
is the highest space-filling efficiency of any sphere-packing arrangement. The nature of extended
structures as well as close-packing, which occurs in two forms called hexagonal close packing
(hcp) and cubic close packing (ccp), will be explored in this lab activity. Sixty-eight of the ninety
naturally occurring elements are metallic elements. Forty of these metals have three-dimensional
submicroscopic structures that can be described in terms of close-packing of spheres. Another
sixteen of the sixty-eight naturally occurring metallic elements can be described in terms of a
different type of extended structure that is not as efficient at space-filling. This structure occupies
only 68% of the available space in the unit cell. This second largest subgroup exhibits a sphere
packing arrangement called body-centered cubic (bcc).

You should be able to calculate the % of void space using simple geometry.

Packing of more than one type of ion (binary compounds) in a crystal lattice

A very useful way to describe the extended structure of many substances, particularly ionic
compounds, is to assume that ions, which may be of different sizes, are spherical. The structure
then is based on some type of sphere packing scheme exhibited by the larger ion, with the smaller
ion occupying the unused space (interstitial sites). In structures of this type, coordination number
refers to the number of nearest neighbors of opposite charge. Salts exhibiting these packing
arrangements will be explored in this lab activity.

Coordination number and interstitial sites

When spherical objects of equal size are packed in some type of arrangement, the number of
nearest neighbors to any given sphere is dependent upon the efficiency of space filling. The
number of nearest neighbors is called the coordination number and abbreviated as CN. The sphere
packing schemes with the highest space-filling efficiency will have the highest CN. Coordination
number will be explored in this lab activity. A useful way to describe extended structures, is by
using the unit cell which as discussed above is the repeating three-dimensional pattern for
extended structures. A unit cell has a pattern for the objects as well as for the void spaces. The
remaining unoccupied space in any sphere packing scheme is found as void space. This void space
occurs between the spheres and gives rise to so-called interstitial sites.

Synthesis of solid state materials

There exist many synthetic methods to make crystalline solids. Traditional solid state chemical
reactions are often slow and require high temperatures and long periods of time for reactants to
form the desire compound. They also require that reactants are mixed in the solid state by
grinding two solids together. In this manner the mixture formed is heterogeneous (i.e. not in the
same phase), and high temperatures are required to increase the mobility of the ions that are being
formed into the new solid binary phase. Another approach to get solid state binary structures is
using a precursor material such as a metal carbonate, that upon decomposition at high
temperatures loses gaseous resulting in very fine particles of the corresponding metal oxide
(e.g., ).

X-ray crystallography

To determine the atomic or molecular structure of a crystal diffraction of X-rays is used. It was
observed that visible light can be diffracted by the use of optical grids, because these are arranged
in a regular manner. Energy sources such as X-rays have such small wavelengths that only “grids”
the size of atoms will be able to diffract X-rays. As mentioned before a crystal has regular
molecular array, and therefore it is possible, to use X-ray diffraction to determine the location of
the atoms in crystal lattice. When such an experiment is carried out we say that we have
determined the crystal structure of the substance. The study of crystal structures is known as
crystallography and it is one of the most powerful techniques used today to characterize new
compounds. You will discuss the principles behind X-ray diffraction in the lecture part of this
course.

Superconductors

A superconductor is an element, or compound that will conduct electricity without resistance

when it is below a certain temperature. Without resistance the electrical current will flow
continuously in a closed loop as long as the material is kept below an specific temperature. Since
the electrical resistance is zero, supercurrents are generated in the material to exclude the
magnetic fields from a magnet brought near it. The currents which cancel the external field
produce magnetic poles opposite to the poles of the permanent magnet, repelling them to provide
the lift to levitate the magnet. In some countries (including USA) this magnet levitation has been
used for transporation. Specifically trains can take advantage of this levitation to virtually
eliminate friction between the vehicle and the tracks. A train levitated over a superconductor can
attain speeds over 300 mph!

Solid State Model Kits

In this experiment we will use the Institute for Chemical Education (ICE) Solid-State Model Kits
which are designed for creating a variety of common and important solid state structures. Please
be careful with these materials as they are quite expensive. There is a list of kit components on the
inside of the lid of each box. Please make sure that you have all the listed pieces and that these are
in their proper locations when you finish using the kit.

The TAs will deduct points from your lab grade if the kits are not returned with all pieces present
and properly organized.

Use of the Solid State Model Kit:

The following instructions are abbreviated. Please consult the instruction manual found in the kits
for more details if you need assistance in building any of the structures given. Note that some of
the model kits are older than others and the manuals’ and page numbers may not correspond.

There are four major part types in each model kit:

*2 off-white, thick plastic template bases with holes (one with a circle, the other a semicircle);

*cardboard templates (about 20 labeled A-T);

*metal rods (to be inserted in the holes to support the plastic spheres)

*plastic spheres in 4 sizes and colors.

The spheres can represent atoms, ions, or even molecules depending upon the kind of solid it is.

You will be given directions for the use of a specific base, template, placement of the rods,
selection of spheres, and arrangement of the spheres as you progress. The ICE model kits make
use of Z-diagrams to represent how the structure will be built up. Each type of sphere will be
numbered with the z layer in which it belongs.
As we build each structure in three-dimensional space, we will be drawing figures to represent the
unit cell structures. Each level or layer of atoms, ions, or molecules in a unit cell can be
represented by a two-dimensional base, that is, a square, hexagon, parallelogram, etc.

To draw the Z-diagrams the bottom layer is referred to as z=0. We then proceed layer by layer up
the unit cell until we reach a layer which is identical to the z=0 layer. This is z=1. Since z=0 and
z=1 are identical by definition, we do not have to draw z=1, although you might want to do so as
you are learning how to work with solid state figures. The layers between top and bottom are
given z designations according to their positions in the crystal. So, for example, a unit cell with 4
layers (including z=0 and z=1) would also have z=0.33 (1/3) and z=0.67 (2/3).

Each solid-state kit has two types of bases (one using rectangular coordinates, the other using
polar coordinates) indicated by a full circle or semicircle, or by color (yellow and green.)

You will first build structures that involve only one type of atom, as you would find in crystalline
solids of the elements, especially that of the metals. Then you will examine ionic compounds
which are known as binary solids. Binary solids are those composed of only two types of atoms,
such as sodium chloride or calcium fluoride.

If time permits there is an extra credit exercise you can do. You may not do this extra credit
exercise until the report form has been completed nor may you receive credit for the extra credit
assignment unless you fully complete the report form.

Working groups and teams

You and your lab partner will constitute a group. Each group will receive one model kit and two
groups will work together as a team. Your TA will assign you the structures you have to do, and at
the end each team will discuss the structures assigned on front of the class. The number of teams
and the assignments the TA will give you will be decided based on the number of students in a
particular laboratory session. The laboratory is divided for six teams (A-F)

Experimental Procedure

Every part of the experimental procedure has correspondent questions on the Report Form. Do not
proceed until ALL questions accompanying each section have been answered and recorded.

1. Demonstration of the 1,2,3-superconductor

A pellet of the 1,2,3-superconductor is placed on the top of an inverted paper cup. The
pellet is cooled down by carefully pouring liquid nitrogen over it until the bottom of the cup is
filled up. After approximately 10 seconds (when the bubbling stops) the pellet should reach the
liquid nitrogen temperature. Your TA will then place a very strong magnet over the pellet.
What happens to the magnet? What happens as the superconductor warms up? What is the
Meissner effect? (Write observations and answer these questions on your report form)

Warning- LIQUID NITROGEN CAN CAUSE FROST BITE! Do not directly touch anything that
has come into contact with the liquid nitrogen until it is warmed up to room temperature.

NOTE TO TA: to remove a levitating magnet, simply wait until the liquid nitrogen fully
evaporates or use another magnet to "grab" the floating magnet. Be careful not to lose or break
these very tiny, yet expensive, magnets!!!!

2. Cubic Cells

There are many types of fundamental unit cells, one of which is the cubic cell. In turn, there are
three subclasses of the cubic cell:

a. simple or primitive cubic (P)

b. body-centered cubic (bcc, I*)

c. face-centered cubic (fcc, F)

*The I designation for body-centered cubic comes from the German word innenzentriert.

We do not have time to build models of all of the unit cells possible, so we will focus on the cubic
structure and its variations. Our investigation will include several aspects of each cell type:

the number of atoms per unit cell

the efficiency of the packing of atoms in the volume of each unit cell

the number of nearest neighbors (coordination number) for each type of atom

the stoichiometry (atom-to-atom ratio) of the compound

A. Simple Cubic Unit Cells or Primitive Cubic Unit Cells (P)

Team A

Group 1. Single Unit Cell

· Construct a simple cubic cell using template A and its matching base.

· Insert rods in the 4 circled holes in the shaded region of the template.

· Build the first layer (z = 0) by placing a colorless sphere on each rod in the shaded region.

· Draw a picture of this layer as previously described.

· Complete the unit cell by placing 4 colorless spheres on top of the first layer.

This is the z=1 layer.

Group 2. Extended Structure

Construct an extended cubic cell using template A.

Insert rods in the circled holes of template A in the area enclosed by the dotted lines.

Construct a set of unit cells as described for making a single unit cell.

Look closely at the structures generated by both groups. They are called simple (or primitive)
cubic.

Considering all of the cells around it, answer the corresponding questions on the report form.

B. Body-Centered Cubic Structure (BCC)

Team B

Group 1. Single Unit Cell

· Construct a body-centered cubic (bcc) structure using template F. · Insert the rods in all 5 of the
holes in the shaded region.

· Use the guide at left and place four colorless spheres in the first layer (1) at the corners for z=0.

· Place one colorless sphere in the second layer (2) on the center rod for z=0.5

· Construct the z=1 layer.

Group 2.Extended Structure

Using template F, construct an extended body-centered cubic structure.

Insert rods in every hole of the template/block.

 Using the guide which follows, place colorless spheres for z=0 on every rod labeled 1.

For z=0.5 place colorless spheres on each rod labeled 2.

Complete the z=1 layer and then place another two layers on top.

1. Face-Centered Cubic (FCC) Structure

Team C

Group 1. Single Unit Cell

· Construct a single face-centered cubic cell using template C, colorless spheres and the layering
as illustrated. Only put rods and spheres on one of the squares defined by the internal lines.

Figure 8.1.

Group 2. Extended Structure

· Construct an extended face-centered cubic structure using template C (You can find instructions
on how to do it in the manual that comes with the kit.)

3. Close-Packing: Sphere Packing & Metallic Elements

Team D

Group 1. Construct the hexagonal close-packing unit cell (use the one requiring the C6 template)

Group 2. Construct the cubic close-packing unit cell (use the one requiring the C6 template)

Team E
Group 1. Add a 2' layer on top of the existing structure.

Group 2. Add a 2' layer on top of the existing structure.

Team F

Using only the shaded portion on the template, construct the face-centered cubic unit cell which
uses the C4 template.

Compare the structures of the face-centered cubic unit cell made on the C4 template to that made
on the C6 template.

4. Interstitial sites and coordination number (CN)

Team A

Group 1 - Construct CN 8, CN 6 and CN 4 (using the C4 template).

Group 2 - Construct CN 6, CN 4 (body diagonal) (using the C6 template).

5. Ionic Compounds

Now we will look at some real ionic compounds which crystallize in different cubic unit cells. We
will use the models to determine the stoichiometry ( atom-to-atom ratios) for a formula unit.

Team B

Cesium Chloride

· Construct a model of cesium chloride on template A. This time use colorless spheres as layers 1
and 1' and the green spheres for layer 2.

· Start with the shaded area and then work your way outward to an extended structure. Consider
both simple and extended structures when answering the questions which follow.

Team C

Fluorite: Calcium fluoride

· Construct a model of fluorite, which is calcium fluoride, on template E.

· Green spheres will be used for layers 1, 3, and 1' while colorless spheres go on layers 2 and 4.

· Finish with a 1' layer on top. Build the structure by placing rods in all 13 holes in the area
enclosed by the internal line.

Team D

Lithium Nitride

· Use the L template and insert 6 rods in the parallelogram portion of the dotted
lines.

· Construct the pattern shown below. Be sure to include a z=1 layer. 1 is a green
sphere while 1 and 2 are blue spheres. The 0 indicates a 4.0 mm spacer tube; the
2 is an 18.6 mm spacer.

Figure 8.2.

Teams E and F

Zinc Blende and Wurtzite: Zinc Sulfide

Team E. Zinc Blende: Use template D to construct the crystal pattern illustrated below. Numbers 2
and 4 are blue spheres while 1 and 3 are colorless spheres and 4 is a 16.1 mm spacer.

Team F. Wurtzite: Use template L to construct the Wurtzite lattice. Numbers 1, 3 and 1' are
colorless spheres and Numbers 2 and 4 are pink spheres.

Figure 8.3.

Pre-Lab: Solid State and Superconductors

(Total 10 Points)
Hopefully here for the Pre-Lab

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

1. List the existing crystal systems (unit cell types):

2. Which of these unit cells will we study in this laboratory exercise?

3. Which are the three subclasses of this type of unit cell?

4. Define coordination number:

5. What is the volume of a sphere? Of a cube?

Report: Solid State and Superconductors
Hopefully here for the Report Form

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Part I Demonstration and Unit cell theory

A. TA Demo of the superconductor

Describe and explain your observations (What happens with the magnet? Briefly describe the
Meissner effect?)

B. The unit cell 1. A cube (see below) has _______ corners, _______ edges & _______ faces.

Figure 8.4.

2. Structure A below shows how a unit cell may be drawn where one choice of unit cell is shown
in bold lines. In Structures B, C and D below, draw the outline(s) of the simplest 2-D unit cells
(two-dimensional repeating patterns depicted by a parallelogram that encloses a portion of the
structure).

If the unit cell is moved in the X,Y-plane in directions parallel to its sides and in distance
increments equal to the length of its sides, it has the property of duplicating the original structural
pattern of circles as well as spaces between circles. Can a structure have more than one type of
unit cell? ________
 Figure 8.5.

Table 8.2.

Structure A Structure B Structure C Structure D

3. If the circle segments enclosed inside each of the bold-faced parallelograms shown below were
cut out and taped together, how many whole circles could be constructed for each one of the
patterns:

Figure 8.6.

Table
8.3.

4. Shown below is a 3-D unit cell for a structure of packed spheres. The center of each of 8 spheres
is at a corner of the cube, and the part of each that lies in the interior of the cube is shown. If all of
the sphere segments enclosed inside the unit cell could be glued together, how many whole
spheres could be constructed?

number of whole spheres: ________

5. For each of the figures shown below, determine the number of corners and faces. Identify and
name each as one of the regular geometric solids.
 Figure 8.7.

AB

Table 8.4.

A B

Number of corners

Number of faces

Name of the shape of this object

Part II Experimental

1. Cubic Cells

A. Simple Cubic Unit Cells or Primitive Cubic Unit Cells (P)

a. How would you designate the simple cube stacking - aa, ab, abc, or some other?

b. If the radius of each atom in this cell is r, what is the equation that describes the volume of the
cube generated in terms of r? (Note that the face of the cube is defined by the position of the rods
and does not include the whole sphere.)

c. Draw the z-diagram for the unit cell layers.

d. To how many different cells does a corner atom belong? What is the fractional contribution of a
single corner atom to a particular unit cell?

e. How many corner spheres does a single unit cell possess?

f. What is the net number of atoms in a unit cell? (Number of atoms multiplied by the fraction
they contribute)

g. Pick an interior sphere in the extended array. What is the coordination number (CN) of that
atom? In other words, how many spheres are touching it? .

h. What is the formula for the volume of a sphere with radius r?

i. Calculate the packing efficiency of a simple cubic unit cell (the % volume or space occupied by
atomic material in the unit cell). Hint: Consider the net number of atoms per simple cubic unit
cell (question g) the volume of one sphere (question i), and the volume of the cube (question b).

B. Body-Centered Cubic (BCC) Structure

a. Draw the z diagrams for the layers.

b. Fill out the table below for a BCC unit cell

Table 8.5.

Atom type Number Fractional Contribution Total Contribution Coordination Number

Corner

Body

c. What is the total number of atoms in the unit cell?

d. Look at the stacking of the layers. How are they arranged if we call the layers a, b, c, etc.?

e. If the radius of each atom in this cell is r, what is the formula for the volume of the cube
generated in terms of the radius of the atom? (See diagrams below.)

f. Calculate the packing efficiency of the bcc cell: Find the volume occupied by the net number of
spheres per unit cell if the radius of each sphere is r; then calculate the volume of the cube using r
of the sphere and the Pythagoras theorem ( a2+b2=c2) to find the diagonal of the cube.
 C. The Face Centered Cubic (FCC) Unit Cell

a. Fill out the following table for a FCC unit cell.

Table 8.6.

Atom type Number Fractional Contribution Total Contribution Coordination Number

Corner

Face

b. What is the total number of atoms in the unit cell?

c. Using a similar procedure to that applied in Part B above; calculate the packing efficiency of
the face-centered cubic unit cell.

1. Close-Packing

a. Compare the hexagonal and cubic close-packed structures.

b. Locate the interior sphere in the layer of seven next to the new top layer. For this interior
sphere, determine the following:

Table 8.7.

Number of touching spheres: hexagonal close-packed (hcp) cubic close-packed (ccp)

on layer below

on the same layer

 on layer above

TOTAL CN of the interior sphere

c. Sphere packing that has this number (write below) of adjacent and touching nearest neighbors is
referred to as close-packed. Non-close-packed structures will have lower coordination numbers.

d. Are the two unit cells the identical?

e. If they are the same, how are they related? If they are different, what makes them different?

f. Is the face-centered cubic unit cell aba or abc layering? Draw a z-diagram.

III.Interstitial sites and coordination number (CN)

a. If the spheres are assumed to be ions, which of the spheres is most likely to be the anion and
which the cation, the colorless spheres or the colored spheres? Why?

b. Consider interstitial sites created by spheres of the same size. Rank the interstitial sites, as
identified by their coordination numbers, in order of increasing size (for example, which is
biggest, the site with coordination number 4, 6 or 8?).

c. Using basic principles of geometry and assuming that the colorless spheres are the same anion
with radius r A in all three cases, calculate in terms of rA the maximum radius, rC, of the cation
that will fit inside a hole of CN 4, CN 6 and CN 8. Do this by calculating the ratio of the radius of
to cation to the radius of the anion: rC/rA.

d. What terms are used to describe the shapes (coordination) of the interstitial sites of CN 4, CN 6
and CN 8?
CN 4: ________________

CN 6: _______________

CN 8: ________________

IV.Ionic Solids

A. Cesium Chloride

1. Fill the table below for Cesium Chloride

Table 8.8.

Colorless spheres Green spheres

Type of cubic structure

Atom represented

2. Using the simplest unit cell described by the colorless spheres, how many net colorless and net
green spheres are contained within that unit cell?

3. Do the same for a unit cell bounded by green spheres as you did for the colorless spheres in
question 4.

4. What is the ion-to-ion ratio of cesium to chloride in the simplest unit cell which contains both?
(Does it make sense? Do the charges agree?)

B. Calcium Fluoride
1. Draw the z diagrams for the layers (include both colorless and green spheres).

2. Fill the table below for Calcium Fluoride

Table 8.9.

Colorless spheres Green spheres

Type of cubic structure

Atom represented

3. What is the formula for fluorite (calcium fluoride)?

C. Lithium Nitride

1. Draw the z diagrams for the atom layers which you have constructed.

2. What is the stoichiometric ratio of green to blue spheres?

3. Now consider that one sphere represents lithium and the other nitrogen. What is the formula?

4. How does this formula correspond to what might be predicted by the Periodic Table?

D. Zinc Blende and Wurtzite

Fill in the table below:

Table 8.10.

Zinc Blende Wurtzite

Stoichiometric ratio of colorless to pink spheres

Formula unit (one sphere represents and the other the sulfide ion)

Compare to predicted from periodic table

Type of unit cell

Solutions
 Chapter 9. Organic Reactions

Organic Reactions

Objectives

Synthesis of some important esters.

Oxidation of a primary alcohol first to an aldehyde and then a carboxylic acid.

To saponify a typical vegetable oil.

Grading

You will be assessed on

detailed answers required in the lab report.

the correctness and thoroughness of your observations.

Introduction

Esters are an important class of organic compounds commonly prepared from the esterification
reaction of an organic acid with an alcohol in the presence of a strong mineral acid (usually
). They are chiefly responsible for the pleasant aromas associated with various fruits, and as such
are used in perfumes and flavorings. Some esters also have useful physiological effects. The best
known example is the analgesic ("pain killing") and anti-pyretic ("fever reducing") drug
acetylsalicylic acid, otherwise known by its trade name aspirin.

Liniments used for topical relief of sore muscles contain the ester methyl salicylate ("oil of
wintergreen"), which is prepared from the reaction of methyl alcohol with the acid group of
salicylic acid. Methyl salicylate acts as an analgesic and is absorbed through the skin; however,
methyl salicylate is also a skin irritant (like many organic substances), which in this instance
provides the beneficial side effect of the sensation of warming in the area of the skin where the
liniment is applied.

Oxidation of a primary alcohol may yield either an aldehyde or a carboxylic acid, depending on
the reaction conditions. For example, mild oxidation of ethanol produces acetaldehyde, which
under more vigorous conditions may be further oxidised to acetic acid. The oxidation of ethanol to
acetic acid is responsible for causing wine to turn sour, producing vinegar.
A number of oxidising agents may be used. Acidified sodium dichromate (VI) solution at room
temperature will oxidise primary alcohols to aldehydes and secondary alcohols to ketones. At
higher temperatures primary alcohols are oxides further to acids.

Figure 9.1.

The dichromate solution turns from the orange color of the (aq) to the blue color of the
(aq). This color change is the basis for the "breathalyser test". The police can ask a motorist
to exhale through a tube containing some orange crystals. If the crystals turn blue, it shows that
the breath contains a considerable amount of ethanol vapor.

Soaps are produced by the reaction of metallic hydroxides with animal fats and vegetable oils. The
major components of these fats and oils are triglycerides. Triglycerides are esters of the
trihydroxy alcohol called glycerol and various long-chain fatty acids. Tristearin is a typical
triglyceride. Upon reaction with sodium hydroxide, the ester bonds of tristearin are broken. The
products of the reaction are the soap, sodium stearate, and glycerol. This type of reaction is called
saponification (Greek: sapon, soap) and it is depicted below.

Figure 9.2.

Soap is made commercially by heating beef tallow in large kettles with an excess of sodium
hydroxide. When sodium chloride is added to this mixture (called the "saponified" mixture), the
sodium salts of the fatty acids separate as a thick curd of crude soap. Glycerol is an important by-
product of the reaction. It is recovered by evaporating the water layer. The crude soap is purified,
and coloring agents and perfumes are added to meet market demands.

EXPERIMENTAL PROCEDURE

CAUTION WEAR EYE PROTECTION!

CAUTION - Concentrated sulfuric acid will burn and stain the skin as well as damage clothing. In
case of skin or clothing contact, wash the area immediately with large amounts of water.

Synthesis of esters

1. Place approximately 2 g (or 2 mL if the substance is a liquid) of the organic acid and 2 mL of
the alcohol in a large test tube.

2. Add 5 - 7 drops of concentrated (18 M) sulfuric acid, mix the solution well with a glass
stirring rod and then place the test tube in a hot water bath (largest beaker in your drawer) (~
80°C) for 5 - 10 minutes.

3. Remove the test tube from the hot water bath and cautiously pour the mixture into about 15
mL of saturated sodium bicarbonate contained in a small beaker. The sodium bicarbonate will
destroy any unreacted acid.

4. Observe the aroma produced from each of the following esterification reactions. Write the
structure of the esters produced, and the balanced equations for the esterification and the
acid/sodium bicarbonate reactions:

Complete the following reactions using the procedure above and record your observations.

(1)

salicylic acid + methyl alcohol

(2)

1 - octanol + glacial acetic acid

(3)
amyl alcohol + glacial acetic acid

(4)

ethanol + acetic acid

Oxidation of an alcohol with acidified potassium dichromate(VI) solution

Add 10 drops of dilute sulfuric acid (6M) and 5 drops of potassium dichromate(VI) solution
(0.01M) to 5 drops of ethanol. The oxidising agent is added slowly to the alcohol so that the
temperature is kept below that of the alcohol and above that of the carbonyl compound.
(Carbonyl compounds are more volatile than the corresponding alcohols). Usually the alcohol
is in excess of the oxidant and the aldehyde is distilled off to avoid further oxidation.

Note the color and smell cautiously (Royal Wave).

Warm the mixture and smell cautiously (Royal Wave).

Repeat the experiment using first methanol and then propan-2-ol in place of ethanol.

Describe what happens and explain the color changes.

What conditions and techniques would favour the oxidation of ethanol to

a. ethanal rather than ethanoic acid.

b. ethanoic acid rather than ethanal?

Oxidation of an alcohol with acidified potassium permanganate (VII) solution

Add 10 drops of dilute sulfuric acid and 5 drops of potassium permanganate (VII) solution
(0.01M) to 5 drops of ethanol. Note the color and smell cautiously.

Warm the mixture and smell cautiously (Royal Wave).

Repeat the experiment using first methanol and then propan-2-ol in place of ethanol.

Take the pH of your final mixture using Universal indicator paper

Describe what happens and explain the color changes.

What is your final product?

Saponification of a vegetable oil

CAUTION - Sodium hydroxide is a very caustic material that can cause severe skin burns. Eye
burns caused by sodium hydroxide are progressive: what at first appears to be a minor irritation
can develop into a severe injury unless the chemical is completely flushed from the eye. If sodium
hydroxide comes in contact with the eye, flush the eye with running water continuously for at least
20 minutes. Notify your TA immediately. If sodium hydroxide is spilled on some other parts of
the body, flush the affected area with running water continuously for at least 2-3 minutes. Notify
your TA immediately.

Never handle sodium hydroxide pellets with your fingers. Use weighing paper and a scoopula.
Solid sodium hydroxide will absorb water from the atmosphere. It is hygroscopic. Do not leave
the container of sodium hydroxide open.

Keep ethanol and ethanol-water mixtures away from open flames.

Aqueous iron chloride will stain clothes permanently and is irritating to the skin. Avoid contact
with this material.

In this experiment, you will saponify a vegetable oil

1. Pour 5 mL (5.0 g) of vegetable oil into a 250-mL beaker.

2. Slowly dissolve 2.5 g of NaOH pellets in 15 mL of the 50% ethanol/water mixture in a 50-mL
beaker.

3. Add 2-3 mL of the NaOH solution to the beaker containing the oil. Heat the mixture over a hot
plate with stirring. CAUTION: Keep your face away from the beaker and work at arm's length.
Stirring is required to prevent spattering. Every few minutes, for the next 20 minutes, add
portions of the ethanol/water mixture while continuing to stir to prevent spattering. After
about 10 more minutes of heating and stirring, the oil should be dissolved and a homogenous
solution should be obtained.

4. Add 25 mL of water to the hot solution. Using the hot grips, pour this solution into a 250 mL
beaker containing 150 mL of saturated NaCl solution. Stir this mixture gently and permit it to
cool for a few minutes.

5. Skim the soap layer off the top of the solution and place it in a 50-mL beaker.

6. Into a test tube, place a pea-sized lump of your soap. Place a similar amount of laundry
 detergent in a second tube and a similar amount of laundry detergent in a second tube and a
similar amount of hand soap in a third tube. Add 10 mL of water to each tube. Stopper each
tube and shake thoroughly.

7. Estimate the pH of the solution using wide-range indicator solution or wide-range test paper.
Record the results. Pour the contents of the test tubes into the sink and rinse the tubes with
water.

Figure 9.3.

Pre-Lab: Introductory Organic Reactions

(Total 25 Points)
Hopefully here for the Pre-Lab

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

This assignment must be completed individually and turned in to your TA at the beginning of lab.
You will not be allowed to begin the lab until you have completed this assignment.

For questions 1-4, draw the structural formulae of:

1) 2,2 - dimethylbutane

2) 3-ethyl-2,4-dimethylpentane

3) 2,3,4-trimethylhexane
4) 3-ethyl-2-methylheptane

For questions 5-8, give the names of

5)

6)

7)

8)

For questions 9-11, give the structural formulae for:

9) hex-3-ene

10) 3-methylhex-1-ene
11) 2,5- dimethylhex-2-ene

For questions 12-14, give the names of:

12)

Figure 9.4.

13)

Figure 9.5.

14)

Figure 9.6.

For questions 15-19, give the stuctural formulae of:

15) trans-1,2-dibromoethene

16) trans-1-chloroprop-1-ene

17) cis- hex-2-ene

18) pent-1-yne

19) 3-methylbut-1-yne

For questions 20-25, name the following compounds:

20)

Figure 9.7.

21)

Figure 9.8.

22)

Figure 9.9.

23)

Figure 9.10.

24)
 Figure 9.11.

25)

Figure 9.12.

Report: Organic Reactions

Hopefully here for the Report Form

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Observations:

Synthesis of esters

Table 9.1.

Reagents Product Observations

C7H6O3(salicylic acid ) + (methyl alcohol)

(1 - octanol ) (glacial acetic acid)

(amyl alcohol) (glacial acetic acid)

 (ethanol) (acetic acid)

Oxidation of an alcohol with acidified potassium dichromate(VI) solution.

Remember to describe what happens and explain the color changes.

What conditions and techniques would favour the oxidation of ethanol to

a. ethanal rather than ethanoic acid.

b. ethanoic acid rather than ethanal?

Table 9.2.

Observations:
Add 10 drops of dil. to 5 drops of Observations: color/smell on
color/smellSmell
to the following alcohols warmingSmell cautiously!
cautiously!

Ethanol

Methanol

Propan-2-ol

Oxidation of an alcohol with acidified potassium permanganate (VII) solution

Remember to describe what happens and explain the color changes.

What is your final product?

Table 9.3.

Observations:
Add 10 drops of dil. to 5 drops Observations: color/smell on
color/smellSmell
of to the following alcohols warmingSmell cautiously!
cautiously!

Ethanol

Methanol
Propan-2-ol

Saponification of a vegetable oil

Table 9.4.

Reagent pH from indicator paper

Your soap

Laundry Detergent

Hand Soap

w from the File menu, and then double-click your template.

Solutions
 Chapter 10. Transition Metals

Transitions Metals: Synthesis of an Inorganic Compound (trans-

dinitrobis(ethylenediamine)cobalt(III) nitrate)

Objectives

To synthesize a transition metal complex of cobalt three, Co(III), and ethylenediamine.

To characterize the resulting metal complex spectroscopically.

To understand concept of limiting reactant.

Grading

Your will be determined according to the following:

prelab (10%)

lab report form (80%)

TA points (10%)

Introduction

The transition metals are the largest “group” (classification) of elements from the periodic table.
These can be found in nature as ores or in its elemental form, such as gold. All transition metals
have more than one oxidation state. Most transition metals (TMs) can complex with other species
(called ligands in “TM Complex” jargon) by giving their electrons to them, forming a complex.
These ligands, which are the nearest neighbor atoms to the metal center, constitute the inner (or
first) coordination sphere. Complexes may be either neutral or charged and have distinctive
properties that may be quite unlike those associated with their constituent molecules and ions,
each of which is capable of independent existence. An example of a charged complex is
ferricyanide, . The and ions found in the ferricyanide complex ion exist as
independent species and in other compounds. The transition metals are well known for forming a
large number of complex ions. In this experiment we will synthesize a transition metal complex
containing cobalt, Co(III), and ethylenediamine.
Stereochemistry

The most common coordination numbers (the number of individual ligands bound) are two, four,
and six, with geometries illustrated in Fig 1:

Figure 10.1.

Fig 1. Common geometries for complex ions. (A) linear, (B) square planar, (C) tetrahedral, and
(D) octahedral

Complexes of Cu(I), Ag(I), Au(I) and some of Hg(II) form linear structures (A) such as ,
, etc. Four-fold coordination (C) is not too common with transition metals, and the square
planar geometry (B) occurs in complexes of Pd(II), Pt(II), Ni(II), Cu(II), and Au(III). Six-fold
coordination (D) is the most common and in fact the one we will study in this laboratory exercise.

A ligand that is capable of occupying only one position in the inner coordination sphere by
forming only one bond to the central atom is called a monodentate (“one tooth”) ligand. Examples
are F−, , , H2O, and . If the ligand has two groups that are capable of bonding to
the central atom, it is called a bidentate ("two teeth") ligand, and so forth. An example of a
bidentate ligand is ethylenediamine , which is commonly abbreviated "en". Both
nitrogen atoms in "en" can bond to the central atom in a complex at the same time.

Complex ion salts with the same chemical formulas often behave differently because the same
number of atoms can be arranged into different forms called isomers. Hydrate isomerism is
illustrated by the following example: There are three distinct compounds with the formula
. One of these, violet in color, reacts immediately with to precipitate all of the
chlorines as AgCl. The second is light green but only ⅔ of the chlorine is precipitated as AgCl.
The third compound is dark green and only ⅓ of the chlorine is precipitated as AgCl. The last
compound has only one reactive Cl, so apparently two chlorines in this compound are bonded
tightly to the Cr and are not available for reaction. We might thus write this compound as
, where the species within the brackets are regarded as ligands bonded fairly
strongly to the central chromium, and this species would behave as a single ion in solution. i.e., in
aqueous solution,

The light green compound with two reactive chlorines is apparently , while the
violet compound with three reactive chlorines is .

Closely related to hydrate isomerism is ionization isomerism, where an ion takes the place of
water. Consider two different compounds with the formula . One of these,
, appears red, whereas the other, , appears violet.

In addition to these coordination sphere isomers there are geometrical isomers, which have
coordination spheres of the same composition but different geometrical arrangement. Geometrical
isomers are distinct compounds and can have different physical properties (although often not too
different) such as color, crystal structure, melting point, and so on. For example, dichlorodiamine
platinum (II) occurs in the square planar geometry (B) so the chlorine ligands can be either next to
one another (cis) or opposite from one another (trans). The compound you will synthesize has an
octahedral geometry with two (bidentate) "en" ligands, and two nitro ligands. The
geometrical isomer you will make is the trans form, in which the ligands are not adjacent to
one another. This difference between cis and trans octahedral isomers is shown in Fig 2.

Figure 10.2.

Fig 2. The trans and cis geometrical isomers for octahedral complexes with two bidentate (“en”)
and monodentate ligands specifically dinitrobis(ethylenediamine)Co(III). The two black
balls represent the ligands and the two pairs of linked white balls represent the two
ethylenediamine ligands. Cis and trans describe the relationship (relative position) between the
two ligands.
In the procedure that follows we start with a cobalt solution made from the salt hexaquacobalt(II)
nitrate, . When this salt dissolves it ionizes to form two ions of and one of
. We wish to prepare a Co(III) compound of ethylenediamine, so we must add
ethylenediamine (en) and oxidize the Co(II) to Co(III). Because Co(II) is more reactive than
Co(III), we allow it to react with (en) first, and then oxidize the resulting complex ion. In aqueous
solution (en) reacts with water to produce ions which can also bind to Co(II), so the pH is
adjusted close to 7 first by adding . (Other acids would introduce new ligands to compete for
the Co.) is added to provide the ligands that will be trans in the final compound. Lastly,
Co(II) is oxidized to Co(III) by bubbling oxygen through the solution.

Experimental Procedure

1. Use your 10 mL graduated cylinder to measure out 20 mL of the 20% by weight solution of
ethylenediamine in dilute .

2. Pour it into a clean 125 mL Erlenmeyer flask. Rinse the graduated cylinder with about 5mL of
deionised water (DI water from white handle faucet) and add the rinse water to the flask. Set
this aside for a moment and prepare the second set of reactants as described below.

3. Weigh out 9.0 g of hexaquacobalt(II) nitrate and 6.0 g sodium nitrite ( ) using a rough
balance (Record mass on report form). Add these reactants to approximately 15 mL of DI
water in an Erlenmeyer flask. After they have dissolved, add the neutralized ethylenediamine
solution prepared in steps 1-2. Record your observations.

4. For the next set of instructions, refer to the diagram below. Fit a piece of rubber tubing over an
inert gas "IG" tap (on benchtop) and open the valve slowly to obtain a gentle flow of oxygen.
Then insert a Pasteur pipet into the other end of the rubber tubing. CAUTION: Too high a gas
flow might blow the pipet out of the tubing and cause serious injury. Always adjust the valve
carefully while pointing your pipet in a safe direction. Test the flow by immersing the pipet tip
in a beaker of water--it should bubble vigorously, but not enough to cause much splashing.
When the flow is set to your satisfaction, immerse the tip of the pipet in the Erlenmeyer flask
containing the reaction mixture. Secure the flask to a stand with a clamp because the reaction
mixture may need about 10 minutes of moderately vigorous bubbling to reach completion.
Record your observations.
 Figure 10.3.

Figure 3. The bubbling apparatus.

1. After about 10 minutes of bubbling, turn off the gas flow and immerse the flask in ice water.
This will cause further crystallization. After approximately 5 minutes in the ice bath, pour the
flask's contents through the filter crucible while it has suction applied using the setup shown
below. Record your observations.

Figure 10.4.

Figure 4. Schematic diagram showing sintered-glass filter crucible mounted on suction flask with
rubber filter adapter. Clamp the filter flask to a support post to prevent breakage.

1. The crystals will remain in the crucible while the solution passes through. Wash your crystals
by slowly pouring approximately 5 mL of ethanol over them while suction is applied. Why do
we wash with ethanol? Answer on lab report form.

2. The next step is recrystallization to obtain a more purified product. Transfer the product
 crystals to a 250 mL beaker. Add about 80 mL of DI water and stir to dissolve the crystals.
Gently heat the beaker over a Bunsen burner (or on high on a hotplate if available), gradually
bringing it to a ‘slight’ boil. Allow the solution to boil gently until its volume has been
reduced to about 50 mL. Then let the solution cooled to near room temperature, place the
beaker into an ice bath (DO NOT PLACE THE BEAKER IN THE ICE BATH WHILE HOT. IT
WILL CRACK AND YOU WILL LOOSE YOUR PRODUCT). Crystal growth should be
immediately apparent. After a few minutes in the ice bath, transfer the crystals into the filter
crucible. To help with this transfer you may use a rubber policeman on the end of a stirring
rod. Remember that your crystals are water-soluble so if you use water in the transfer you will
lose the product. Apply suction and rinse the crystals three times with separate 5 mL portions
of ethanol. Scrape the crystals onto a watch glass and place in your drawer to dry.

In terms of the materials used, the overall reaction is:

However, the actual reaction in solution involves ions and the en species exists partially in the
form of

. From the reaction and quantities used, calculate the theoretical yield and your
percentage yield.

Pre-Lab: Transition Metals

(Total 10 Points)
Hopefully here for the Pre-Lab

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

1. List and draw the common geometries transition metal complexes:

2. What are the two types of structural isomers for complex ion salts?

3. What are the two types of geometrical isomers for complex ion salts?
4. Why do we use Co(II) and then convert to Co(III) when synthesizing ?

5. List two common monodentate ligands and two common bidentate ligands:

Report: Transition Metals

On my honor, in preparing this report, I know that I am free to use references and consult with
others.

Hopefully here for the Report Form

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

Date ________________ Lab Section___________

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students' work (except to compile the group data set) or misrepresent
your own data.

1. Synthesis

A. Volume of 20% ethylenediamine solution used ______ (r = 0.980 g/mL)

Table 10.1.

Compound Weight Moles (Molar weight and stoichiometric coefficient)

ethylenediamine
 a. Observations

1. Record your observations after adding the neutralized ethylenediamine solution.

1. Record your observations after 10 minutes of moderately vigorous bubbling.

2. Record your observations after pouring the flask's contents through the filter crucible while
suction is applied.

b. Questions

1. Why do we wash the crystals with ethanol?

1. Give the net chemical equation for the reaction, writing dissociated reactants as ions, the solid
product as an undissociated salt, and including all other ionic and neutral species needed to
balance charge and mass. Omit any spectator ions that would appear in equally on both sides.

1. Which is the limiting reactant in your experiment?

1. Calculate the maximum weight of product you would have obtained if the limiting reactant
had reacted fully. This is the theoretical yield. What is your percent yield (the actual yield
divided by theoretical yield)?

Theoretical yield _______g Actual yield _______ g

1. Is the yield less, same, or more than the theoretical yield? Give reasons for why the actual
yield is different theoretical yield.

Solutions
 Chapter 11. Physical Properties of Gases

Physical Properties of Gases

Objectives

Learn and understand physical properties of gases and explain observations in terms of the
kinetic molecular theory of gases.

Plot and calculate the root mean square speed of the Carvone molecules. (Comparison with
speed in vacuum).

Estimate volume and volume change of a balloon when it goes from room temperature (RT) to
liquid nitrogen temperature.

Observe and explain behavior of gas in: a soda can, a balloon in a flask, Cartesian diver, etc.,
when a change in pressure or temperature is applied.

Grading

You grade will be determined according to the following:

Pre-lab (10%)

Lab Report Form (80%)

TA points (10%)

Introduction

Expanding and contracting balloons, imploding soda cans, exploding marshmallows are just some
of the demonstrations that are often used to illustrate the empirical gas laws and the kinetic
molecular theory of gases. In this experiment, you will be performing these and other
‘demonstrations’ and using your understanding of the physical properties of gases to explain your
observations.

There will be demonstrations laid out at seven different stations (2 sets at each) around the room
and you will go in 2 groups of 4 people (two sets of lab partners) to each station (you don’t need to
start with #1). If your group is assigned or start with, for example 5, you should then follow the
following order: 5, 6, 7, 1, 2, etc. Your group should spend no more than 15 minutes at each
station. Perform the experiment by following the instructions placed at each station. Then discuss
your observations with your group. For each of the activities, it is important to ask yourself what
is going on, "how can our observations be explained using the kinetic molecular theory of gases?"
Remember that for some demonstrations calculations may be required also. Be thorough and
precise in your explanations.

CAUTION: Important Safety Notes:

Remember to use tongs, hot grips as appropriate when dealing with hot liquids, vapors and
containers.

Liquid nitrogen is extremely cold, with a boiling point of -196 C and if it comes into contact with
skin can result in severe frostbite.

The vacuum dessicator should be regarded as a potential implosion hazard when evacuated.
Handle it carefully.

When doing the egg experiment do not put hot flask immediately in the water bath (let it for at
least 3 minutes sitting on the bench) it will crack and you may have to pay for it if it breaks.

Observe and record what happens in your laboratory report form.

You are encouraged to discuss among yourselves possible explanations to your observations.

Experimental Procedure

Diffusion:

The goal of this experiment is to measure the rate of diffusion of Carvone, a major component of
spearmint oil. Find an area where there are few drafts and the air does not already smell of
spearmint. (You may go to the hallway to perform the experiment)

Stand in a line, with the first person in the group holding the bottle of Carvone and several paper
towels. All four people should be 1 meter apart. You will need to know the distance each person is
from the bottle of Carvone. The fourth person should act as the timekeeper. When the timekeeper
gives the signal, the first person should place a few drops of Carvone on the paper towels. Record
the time that it takes for each person to smell the Carvone. Seal the paper towel in a plastic bag
when you are finished.

After the odor has dissipated, repeat the experiment twice.

Using Excel plot the data in distance traveled versus time. Obtain a least squares fit (R value) for
this data and determine from it the rate of diffusion of Carvone in meters per second. Create a
graph for each trial. Calculate the average of the rates for the three trials. Calculate the root mean
square speed of carvone molecules at 25 C. Your TA will help you with this equation. Compare
the result with the diffusion rate you measured. If they are significantly different, offer an
explanation. Would the diffusion take place faster in a vacuum?

Note: You should spend no more than one-half hour preparing the plots. Please stagger yourselves
so that everyone has an opportunity to get to the computer stations.

Gas Laws in a Soda Can:

Pour 15 mL of water into an aluminum soda can. Set the can on a hot plate and turn on to a high
temperature setting. While the can water heats, fill a 1000-mL beaker with cold water (You may
have a metal tin set out for this purpose). Continue heating the can until the water inside boils
vigorously and until steam escapes from the mouth of the can for about 20 seconds.

Using the hot grips to grip the can near the bottom, quickly lift the can from the burner and invert
(so water covers the mouth of the can) it in the beaker of cold water. Describe what happens.
Explain why it happens. You may repeat this experiment using a second soda can if you wish.
Why is it necessary to invert the can in the water? What would happen if a rigid container were
used?

Balloon in liquid nitrogen:

Review the safety notes above regarding the handling of liquid nitrogen.

Inflate a balloon and tie the end (Several balloons may have already been inflated and tied). Using
tongs, place the balloon in a Dewar flask containing liquid nitrogen. After the balloon stops
changing size, remove it from the Dewar and allow it to warm to room temperature. Observe and
record the changes (you should be able to measure the radius and estimate volume).

Estimate the size of the balloon in liters. What is the pressure inside the balloon before it is placed
in the liquid nitrogen? What is the pressure inside the balloon after it is placed in the liquid
nitrogen? Use the ideal gas law to calculate the percent change in volume expected on going from
room temperature to liquid nitrogen temperature. Is the volume of the cold balloon consistent with
what you calculated, or is it larger or smaller? Suggest an explanation for your observation.
Explain all of your observations in detail using the kinetic molecular theory of gases. How does
the liquid nitrogen cool the gas in the balloon?

Tygon tube in liquid nitrogen:

Review the safety notes above regarding the handling of liquid nitrogen. Place a 2 foot long tygon
clear tube in a Dewar with liquid nitrogen. Observe what happens and explain.
Balloon in a flask:

Place about 5 mL of water in a 125-mL Erlenmeyer flask. Heat the flask on a hot plate until the
water boils down to a volume of about 1 mL. Meanwhile, inflate a balloon and then let the air out
(this may not be necessary if balloons on table have been previously used). Remove the flask from
the heat, hold it with a towel, and immediately place the open end of the balloon over the mouth of
the flask. Observe the effect as the flask cools. Can you get the balloon back out again? If you can,
How?

Cartesian diver:

The Cartesian diver is named for Rene Descartes (1596-1650), noted French scientist and
philosopher. At this station, you will find a plastic soda bottle containing a medicine dropper,
water, and air. Squeeze the bottle.

What happens? Why?

The Egg:

Lightly grease the inside of the neck of a 1 L Erlenmeyer flask with stopcock grease. Clamp the
flask onto the stand. Place about 5 mL H2O in the flask and gently warm it with a Bunsen burner
until the water vaporizes. Do not boil the water to dryness. Meanwhile, prepare an ice water bath
in an evaporating dish. While the flask is warm, seat the egg, narrow end down, in the mouth of
the flask. Unclamp the flask, allow to cool slightly sitting on the bench and then immerse it in the
ice water. (Read the safety notes above to avoid breaking the flask)

Can you get the egg back out again?

Assuming that the flask reaches the maximum vacuum (minimum pressure) possible before the
egg is drawn into the flask, calculate the minimum pressure reached in the flask.

Expanding balloon:

Partially inflate a balloon. Place the balloon inside the vacuum chamber and close the chamber
with the black rubber circle and the top of the chamber carefully centered on the base (A partially
inflated balloon may already be in the dessicator). Close the needle valve (at the bottom of the
black rubber tubing) by turning it clockwise. Turn the stopcock to the up position to connect the
chamber to the vacuum pump. What happens? To open the chamber, turn the stopcock to the left
position and open the needle valve.

Bonus 2 points:
1pt to name a real life example of the physical properties of gases at work

1pt for a good explanation of how and why it works according to what you have learned in the lab.

Pre-Lab: Physical Properties of Gases

(Total 10 Points)
Hopefully here for the Pre-Lab

Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

Name(Print then sign): ___________________________________________________

Lab Day: ___________________Section: ________TA__________________________

1. Define diffusion and write down equation for diffusion rate:

2. Write equation for ideal gas law and describe each term.

3. Define Charles’, Boyle’s, and Avogadro’s law:

4. Fill the blanks (which law applies):

5. When temperature increases in a close balloon the volume ________.

_______Law

When pressure is applied to a close balloon the volume _________.

_______Law

When temperature decreases in a close balloon the pressure _________.

_______Law

Report: Physical Properties of Gases

(Total 80 Points)
Hopefully here for the Report
Note: In preparing this report you are free to use references and consult with others. However, you
may not copy from other students’ work (including your laboratory partner) or misrepresent your
own data (see honor code).

1. Diffusion:

At the end of your report attach the graphs of each trial.

The average of the rates for the three trials is----------------

The root mean square speed of carvone molecules at 25 C is

------------------------------------------------------------------------

Compare the result with the diffusion rate you measured. If they are significantly different, offer
an explanation.

Would the diffusion take place faster in a vacuum?

2. Gas Laws in a Soda Can:

Describe what happens.

Explain why it happens. You may repeat this experiment using a second soda can if you wish.

Why is it necessary to invert the can in the water?

What would happen if a rigid container were used?

3. Balloon in liquid nitrogen:

The estimated size of the balloon in liters is--------------

What is the pressure inside the balloon before it is placed in the liquid nitrogen?

What is the pressure inside the balloon after it is placed in the liquid nitrogen?

Use the ideal gas law to calculate the percent change in volume expected on going from room
temperature to liquid nitrogen temperature.

Is the volume of the cold balloon consistent with what you calculated, or is it larger or smaller?

Suggest an explanation for your observation. Explain all of your observations in detail using the
kinetic molecular theory of gases.

How does the liquid nitrogen cool the gas in the balloon?

4. Balloon in a flask:

What was the effect as the flask cools?

Can you get the balloon back out again?

5. Kissell's tygon tube:

What happens?

Why?

6. Cartesian diver:

What happens?

Why?

7. The Egg:

What happens?

Why?

Can you get the egg back out again?

The minimum pressure reached in the flask is -------------------

8. Expanding balloon:

What happens?

Moore's bonus 2 points:

1pt to name a real life example of the physical properties of gases at work

1pt for a good explanation of how and why it works according to what you have learned in the lab.

Solutions
Index
 Attributions

Collection: Honors Chemistry Lab Fall

Edited by: Mary McHale

URL: http://cnx.org/content/col10456/1.16/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Initial Lab: Avogradro and All That

By: Mary McHale

URL: http://cnx.org/content/m15093/1.1/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Stoichiometry: Laws to Moles to Molarity

By: Mary McHale

URL: http://cnx.org/content/m15095/1.14/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: VSEPR: Molecular Shapes and Isomerism

By: Mary McHale

URL: http://cnx.org/content/m15100/1.8/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Beer's Law and Data Analysis

By: Mary McHale

URL: http://cnx.org/content/m15131/1.3/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Hydrogen and Fuel Cells

By: Mary McHale

URL: http://cnx.org/content/m15192/1.4/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: The Best Table in the World

By: Mary McHale

URL: http://cnx.org/content/m15206/1.2/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Bonding 07

By: Mary McHale

URL: http://cnx.org/content/m15205/1.4/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Solid State and Superconductors

By: Mary McHale

URL: http://cnx.org/content/m15259/1.8/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Organic Reactions

By: Mary McHale

URL: http://cnx.org/content/m15483/1.3/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Transition Metals

By: Mary McHale

URL: http://cnx.org/content/m15503/1.4/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/

Module: Physical Properties of Gases

By: Mary McHale

URL: http://cnx.org/content/m15545/1.7/

Copyright: Mary McHale

License: http://creativecommons.org/licenses/by/2.0/
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