(Lab 1) Measurement and Uncertainty: Density, volume, and propagation of error

Dealing with uncertainty

When we make measurements of the physical world, can we know the true quantity? The accuracy
of a measurement (how close it is to the true value) and the precision of a measurement (how many
significant digits in the quantity) are limited by many factors. For example: how refined is the
equipment or apparatus? How skilled is the observer? Are there inherent physical limitations?
Scientists report not just the quantity and units associated with a measurement, but the uncertainty in
the measurement as well (in this context, the terms error and deviation can be considered
synonyms of uncertainty). For example, the U.S. Mint reports the diameter of a standard quarter
dollar piece as 24.26 mm. What about the uncertainty in the measurement? If the uncertainty is not
provided, we must take a conservative approach in treating the final significant digit and realize this
measurement might be as high as 24.27 mm or as low as 24.25 mm. However, if the measurement had
been reported as 24.2600.005 mm, the measurement would be said to have greater precision.
When we make a measurement, how do we treat its uncertainty? The two types of uncertainty are
referred to as systematic errors and random errors. Systematic errors result from a mis-calibrated
device or a measuring technique that will reliably give a measurement that is too high or too low when
compared with the true value. We typically deal with systematic errors through careful experiment
design. Random errors demand more of our attention and thought. There are three common origins of
random errors we should bear in mind in Chem 125/6, using our best judgment to decide which is
appropriate:
1) Instrument least count. The least count is the smallest division marked on an instrument. Most
meter sticks have a least count of 1/1000th of a meter, or 1.0 mm. An analog wall clock would have a
least count of 1/60th of a minute, or 1.0 s, so a digital stop watch with a least count of 0.02 s would be
more precise by comparison.
2) Estimated error. We have to use conservative judgment when making measurements. For example,
if we have a balance that does not respond to a mass less than 5.0 g while attempting a calibration, we
would have to account for this by estimating the error in any measurement using that balance as
2.5 g (the interval is divided by 2 to reflect a total range, or 5.0 g in this example).
3) Average deviation. We can often deal with random errors in a statistical manner. If we make
repeated measurements several times, we can then find an mean and standard deviation for the dataset.
Both the mean of measurement x (written <x>) and standard deviation (written ) are easily calculated
using software functions. When making repeat measurements, we expect 68% of the values to fall in
the range of (<x> ) to (<x> + ), and 95% of values to fall in the range of (<x> 2) to (<x> + 2).
Example: Five of us measure the density of the same bar of gold, finding the values 19.25 g/mL, 19.33
g/mL, 19.32 g/mL, 19.23 g/mL, and 19.39 g/mL. Using software we find <x> = 19.30 g/mL and =
0.06. Based on these data, we might expect 68% of further trials to give a result in the range of [19.24,
19.36] g/mL. We might also predict that 95% of further trials would give a result in the range of
[19.18, 19.42] g/mL.

Propagation of error
When we use two measurements in a calculation, we are comfortable performing arithmetic on the
quantities: simply add, subtract, multiply, or divide the numbers. When dealing with their
uncertainties, we must be more careful. If we add two measurements of length such as:
24.230.05 mm + 3.660.05 mm = ?

...we can deal with the quantities easily: 27.89. But what of the uncertainties? For addition and
subtraction, we would treat them like this:

0.052 +0.052 = 0.07

...making our new calculated value 27.890.07 mm
Note that in the method shown, the uncertainty is rounded by the rules of significant digits, and the
quantity is rounded to the same decimal place that the uncertainty was.
The general format for addition and subtraction is:

( x)2+( y)2 = z
We call x the uncertainty of measurement x, y is the uncertainty of measurement y, and z is the
uncertainty associated with the new, calculated quantity.
Things change slightly when we multiply or divide measurements. If we want to divide a mass of
3.00.5 kg by a volume of 1.50.2 L, we could once again be quick with the quantity: 2.0 kg/L.
The new uncertainty associated with our answer would be:

z = 2.0 (

0.5
0.2
) +(
) = 0.4
3.0
1.5

making our calculated density 2.00.4 kg/L. Once again, the uncertainty was rounded by the
rules of significant digits, and the quantity was rounded to the same decimal place to match.
The general form for error propagation when multiplying or dividing is:

z = z (

x
y
) +(
)
x
y

Laboratory
Hypothesis:
We can identify the material a regular cube shaped object is composed of based on its density.
Experiment:
Determine the volume of ten different polyhedra supplied in the lab. Use both a standard ruler and a
Vernier caliper and recored the uncertainties in your calculations. Each measurement of a length,
width, height, or mass has an associated uncertainty; when those four quantities are multiplied (or
divided) by each other, we must be careful with how we treat the associated uncertainty (a.k.a. error)
as well. Your work will be evaluated in part based on your written propagation of error for your
conclusions.
Data:
Carefully plan how you want to organize your length, width, height, and mass data for each of your ten
polyhedra. Determine the volume of each mystery polyhedron with both a typical ruler and Vernier
caliper. Recall that density is mass divided by volume, and remember to record the uncertainty for
each measurement you make.
Conclusions:
For your post-lab write-up, what do you think each of your ten cubes is composed of? Compare your
densities (with uncertainty intervals!) to those of published values for common materials. Cite your
sources. How to the measurements made with a typical ruler compare to those made with the Vernier
caliper? Which density measurements have the widest range of uncertainties, your individual
calculations obtained from propagated errors, or the class-wide data complete with standard deviations?

(Lab 2) Determining a Molecular Formula: waters of hydration

Waters of hydration
Chemists use the phrase salt to mean any ionic compound (no net charge) that results from a
neutralization reaction of an acid and a base. Most salts are composed of a metal cation and a nonmetal
anion, and are occasionally encountered as hydrates, meaning they have a number of water molecules
associated with each formula unit of the salt.
One famous example of a hydrate is magnesium sulfate heptahydrate (common name: epsom salts)
whose formula is:
MgSO47H2O
The bullet character followed by a coefficient of seven tells us that there are seven moles of water
associated with every one mole of magnesium sulfate. In this example we might say that there are
seven waters of hydration, which can often be removed from a sample by heating the sample:
magnesium sulfate heptahydrate becomes anhydrous magnesium sulfate above 200 C.
Laboratory
Hypothesis:
We can determine how many waters of hydration are lost from a given hydrate sample by measuring
the mass before and after heating.
Experiment:
You will be assigned a hydrate sample whose formula (including waters of hydration) is known. Your
task is to confidently identify the product obtained upon heating.
Obtain a hydrate sample along with an oven-dried crucible. Your GSI will handle the hot ceramic,
though you will need to record the crucible's mass. Place a measured amount of your solid unknown
hydrate in the crucible. The actual amount you aim to measure is not crucial, anywhere between 1 g
and 2 g will do, as long as you recored the particular mass of hydrate sample that makes it into your
crucible. Return the crucible & hydrate sample to the oven (via your GSI) and heat at
~200 C for 30 minutes.
Your GSI will retrieve your heated crucible + sample from the oven and immediately place it on the
balance you used to obtain the tared mass. Record this new, dehydrated mass of your crucible +
sample.
Data:
The crucial measurements we will make are the mass of your hydrated compound prior to heating, and
the mass of your sample after heating. You will also know the identity of the molecular formula prior
to heating.
One important (but often-overlooked) measurement you should have made is the mass of your ovendried crucible; we sometimes refer to this as the tare or tared mass and it is useful to know in order
to subtract the value from your final mass measurement to determine how much sample remains after
heating.

Conclusions:
For your post-lab write-up the big questions are: compared to your sample's original formula, how
many waters of hydration did it lose, and what is the new formula? Some other things your reader
might want to know: How did you perform your calculations-- can you explain them step by step?
How confident are you in your calculations (or range of possibilities) for your hydrate? Based on inclass conversations with classmates investigating the same starting material, how did your sample
behave compared to theirs? How do your data and conclusions compare with their work?

(Lab 3) The Ideal Gas Law: Calculating the Amount of ATP by Production of CO2 from Glucose and
Yeast
Yeast fermentation is commonly used by humans to produce bread and alcoholic beverages. The yeast
converts sugar to a food source (which we humans consider energy storage). In order to accomplish
this, yeast must have the proper enzymes capable of breaking down sugars in a useful way; that is, to
ferment the sugar. In general, fermentation can be considered a common biological process that occurs
when a sugar is converted to an alcohol, transferring energy from sugar to ATP. Yeast can convert, or
metabolize, sugar both aerobically (with oxygen) and anaerobically (without oxygen). The two
processes generate different products. In both cases, oxidation and reduction of biomolecules occurs.
The aerobic fermentation converting glucose to energy and the production of CO2 can be represented:
C6Hl2O6 (aq) + 6 O2 (g) 6 H2O (l) + 6 CO2 (g) + energy + (36 38 ATP) + heat
And the similar anaerobic fermentation can be represented:
C6Hl2O6 (aq) 2 C2H6O (l) + 2 CO2 (g) + energy + (2 ATP) + heat
The amounts of energy, CO2, and ATP generated depend on the specific conditions. Your task is to
determine how much ATP is produced from glucose in a given sample of yeast cells.
Laboratory
Hypothesis: Using the partial pressures knowledge from the lecture and the Ideal Gas Law (PV = nRT)
you can determine the amount of ATP (from your bakers yeast) that is present based on the amount of
CO2 produced from reduction of the glucose.
Experiment: Fill a large tub with water and dissolve 1 g of citric acid and 1 g of sodium bicarbonate.
This CO2 saturated sample will be used throughout the experiment. Next fill a 10 ml graduated cylinder
with the water and invert it in the tub, and ensure it is completely filled (there may be a small bubble at
the 0 mL line when the cylinder is inverted). Place a piece of tubing into one end of the graduated
cylinder and the other to a rubber stopper adapter. Ensure that your rubber tubing has a minimal amount
of water through the line.
Add 0.20 g of bakers yeast to a small test tube, and suspend the yeast in 2.0 mL warm water (around
26 4 C), and keep this yeast sample warm in an external bath of warm water for 10 minutes. In a
larger test tube, dissolve 0.50 g of glucose in 8.0 mL of warm water (also around 26 4 C). Carefully
place the small test tube into the large one without mixing the two.
Connect the rubber stopper adapter to the top of the large tube and make sure it is now a closed system
from the test tubes to the CO2-saturated water. Begin to mix the 2 test tubes together by gently tilting
the tubes side to side. Keep an eye on the test tubes and the water bath; you should begin to see a
collection of gas bubbles as water is displaced from the graduated cylinder. Gently agitate the test
tubes throughout the reaction sequence to induce more CO2 release.
Data: Once the reaction is complete or slows down to an apparent halt, record the change in volume in
the 10.0 ml graduated cylinder as accurately as possible. Record the time it took for the reaction to slow
down and/or stop. You might experience a peculiar smell if you waft the scent to your nose. What does
it smell like?

Conclusions: Based on the data from this lab, what were the partial pressures of CO2 and water vapor
generated? How much ATP (in moles) was produced in this reaction? What assumptions are you
making when determining this value? (e.g. do you believe the reaction did not go to completion in the
time allotted? What sources of uncertainty are present in your measurements and calculations assuming
that it did?
What was the limiting reactant in this fermentation? Why do you think this is the case? Can anything
be considered a catalyst in this reaction? Why or why not? Was this an anaerobic or aerobic
fermentation process?
How long did your reaction take and how much CO2 was collected? How do these results compare to
the class? If your result were much different from the average, why do you think this occurred? Choose
a parameter of this experiment and propose an alternate outcome if that parameter were changed in a
follow-up experiment, based on your understanding of fermentation. For example, if the same volume
of CO2 was released in this reaction but the pressure in the graduated cylinder was higher than ambient
room pressures, how would your answer for the amount of ATP released change?

(Lab 4) Oxidation & Reduction: exchanging electrons as currency

The ionic charge and the oxidation state of an element in a chemical reaction are closely related, but
they are not the same. Charge is a coulombic phenomenon, and is measurable empirically. Oxidation
states are imaginary human constructs that merely help us organize reactivity patterns in our mind.
Nevertheless, we find oxidation states helpful in deciding when a transfer of electrons has taken place.
In this lab you will determine the relative reactivities of metals through experiment, and be able to
identify the reactants and products of redox reactions.
Laboratory
Hypothesis:
We will be able to rank a series of elements according to their strength as reducing agents or oxidizing
agents. In colloquial terms, we should be able to predict who will reduce whom.
Experiment:
For the first series of experiments we will have the following metals available: Cu, Zn, Mg, Sn
We will also have the following metal ions available: Cu2+, Zn2+, Mg2+, Na+, H+, Sn2+
Our goal as a class is to pair up each of the metals with each of the cations listed and determine in each
case whether a reaction occurs or not.
Your GSI will announce how they wish to assign all 24 combinations among your class groups. In
general, use the metal cations as the provided 0.1 M nitrate solutions. The exception is for Sn2+, which
you should use as SnCl2. For H+ use 1.0 M HNO3.
- Clean each of the metals you plan to use with sandpaper; this will remove any oxide coating on the
surface.
- Use 1 2 mL of each solution in a small test tube, vial, or well plate for observation.
- Allow your mixtures to stand for 30 minutes before making a decision regarding whether or not a
reaction took place.
- If you are having difficulty distinguishing between a no reaction outcome and a sluggish reaction,
you may increase the metal ion concentration by adding crystals of the solid to your 0.1 M solution.
The second series of experiments we will perform three reactions using the sodium iodide each time,
but varying the metal cation present. For each of the following, determine if a redox reaction has taken
place.
Dissolve ca. 0.5 g of solid copper(II)nitrate in 20 mL deionized water. Dissolve ca. 0.5 g of sodium
iodide in a separate 20 mL of deionized water. Pour the two solutions into a third beaker and record
your observations.
Mix 2 mL of 0.1 M sodium iodide and 2 mL hexane. Add 2 mL of 0.1 M iron(III)chloride and shake
well. Record your observations.
Mix 2 mL of 0.1 M sodium iodide and 2 mL hexane. Add 2 mL of 0.1 M tin(IV)chloride and shake
well. Record your observations.
For next week:
You will need to prepare solutions of the following salts for your work next week, and store these
solutions. One liter of each is recommended for your entire lab section to share.

0.1 M potassium nitrate from solid potassium nitrate 0.1 M zinc nitrate from solid zinc nitrate
0.1 M magnesium sulfate from solid magnesium sulfate
0.1 M iron(II) sulfate from solid iron(II) sulfate
0.1 M copper(II) nitrate from solid copper(II) nitrate
1.0 M copper sulfate from solid copper sulfate
Data:
For the reactions you are responsible for testing, if a reaction occurs we gain insight into the relative
reactivity of the participants. For example, if we were to observe:
Zn(s) + Cu2+(aq) Zn2+(aq) + Cu(s)
...we would conclude that Zn is more reactive than Cu (stronger reducing agent), and Cu2+ is more
reactive than Zn2+ (stronger oxidizing agent) since the reaction proceeded to the right as written. If no
reaction occurs, we would conclude the opposite.
Conclusions:
Some ideas to consider for your post-lab write-up:
- How does your class rank the reducing agent strength of the tested metals?
- How does your class rank the oxidizing agent strength of the tested metal ions?
- Compare the ranked reactivities of the tested metals with the ranked reactivities of the tested metal
cations. Is there a pattern? Can you discern a predictable relationship?
- Based on your data, can you predict the relative reducing agent strength of Na and H2?
- For the three reactions you performed with sodium iodide and a varying metal, and based on your
knowledge of likely spectator ions, who is reducing whom? Can you write a net ionic equation for the
reaction you suspect is taking place? What about a balanced molecular equation for each? How sure
are you about the oxidation state of the resulting metal cation? You may find a table of reduction
potentials helpful.

(Lab 5) Galvanic Cells: electrons flowing spontaneously

Introduction
Most of our modern economy and civilization are based on moving electrons in time and space in a
controlled manner. From the macroscale infrastructure of our electrical grid to the microscale of the
circuitry in our mobile phones, we expect electrons to flow where we want them, when we want them.
We will investigate some fundamentals of electron flow in solution phase systems in this lab. Our
emphasis will be on pairing a variety of half-cells to build circuits, and collecting data to characterize
the behavior of our cells.
The term galvanic cell is used to describe a circuit involving the spontaneous transfer of electrons. In
this context, spontaneous has the meaning that once we have mixed two or more chemical species, a
reaction occurs without our further intervention; something in the reaction gains electrons and
something else has lost electrons. Instead of mixing the oxidizing agent and reducing agent in the same
solution, we will prepare a separate solution of each and connect them with a wire. In this way we will
exert some measure of control over where the electrons flow.
The electrode that is supplying the electrons (and hence being oxidized) is called the anode, while the
electrode receiving the electrons (and is itself reduced) is called the cathode. Other components in our
circuit will include a multimeter to measure the cell potential, and a salt bridge to neutralize the ionic
charge that would otherwise build up at each terminal.
Laboratory
Hypothesis:
Through careful observation we can characterize the behavior of galvanic cells and determine the
concentration of an unknown solution sample.
Experiments:
Polish two strips of copper, one strip of zinc, one of magnesium, and one of iron using sandpaper or
steel wool. Rinse these five metal strips with dilute (1.0 M) HNO3 into the proper waste container
(caution!), and again with deionized water. These polished metals will be your electrodes.
Fill one small beaker -full with 0.1 M Zn(NO3)2, a second -full with 0.1 M CuSO4, a third -full
with 0.1 M MgSO4, and a fourth -full with 0.1 M FeSO4. These solutions will be your half-cells.
Place a copper electrode in the CuSO4 solution and the zinc electrode in the Zn(NO3)2 solution. Prepare
a salt bridge by rolling a large piece of filter paper and saturating it with 0.1 M KNO3 solution. Place
one end of the filter paper in each half cell. Connect two leads to the multimeter (one in the COMmon
port, one in the V//mA port), then the probe end of each lead to the electrodes. If you obtain a
negative potential, switch which electrode the leads are contacting. Set the multimeter to the
appropriate range (~2000 mV is a good first guess). Record your measurement, and identify which
electrode is the cathode and which is the anode. Repeat for the other five pairings of half-cells we can
build using these four solutions and electrodes. Remember to prepare a fresh salt bridge for each new
cell.
Construct a cell using your 0.1 M Zn(NO3)2 half-cell paired with the CuSO4 solution of unknown
concentration, measure the cell potential and (assuming the reduction potential of the Zn2+(0.1 M)/Zn
half-cell is 0.76 V) calculate the reduction potential of this unknown Cu half-cell relative to the Zn

half-cell.
Starting with the 1.0 M CuSO4 solution provided, prepare a series of 10-fold dilutions to obtain CuSO4
solutions of 0.1, 0.01, 0.001, and 0.0001 M concentrations. Portions of ca. 35 mL of each solution
should suffice for all experiments.
Set up a galvanic cell using 1.0 M CuSO4 and 0.001 M CuSO4, and immerse a polished copper
electrode in each. Measure the cell potential and determine the cathode and anode. Write an equation
for the reaction occurring in each half-cell.
Set up four more galvanic cells, this time using the Zn/Zn2+ half-cell each time, and pairing it with the
0.1 M. 0.01 M, 0.001 M, and 0.0001 M CuSO4 half-cells in sequence. Make sure to prepare a new salt
bridge each time you change the concentration. You may need to reset the multimeter to a lower range
for these experiments. Record the potential difference for each pairing.
Data:
-For the Cu/Zn, Mg/Zn, and Fe/Zn cells, assume the reduction potential of the Zn2+(0.1 M)/Zn half-cell
is 0.76 V. Determine the reduction potential of the other three half-cells. Do these agree with the
table of standard reduction potentials? How much uncertainty are you therefore dealing with in your
measurements?
-For your Zn vs. Cu cells of varying [Cu2+], compare to the theoretical cell potential from a table of
standard reduction potentials and the Nernst equation. How do things compare from your experimental
values vs. theory? Your instructor will be interested to see your calibration curve plot.
Conclusions:
Can you write balanced equations for the oxidation/reduction reaction that took place in each cell you
constructed? Can you identify the cathode and anode for each? What was the molar concentration of
your unknown solution? For each cell you constructed, which direction did electrons flow? What
about the direction of cations and anions flowing through the salt bridges? For the cell constructed
using to copper electrodes, why did a current flow even though the electrodes were identical?