F24 203 Lab 2 Updated
F24 203 Lab 2 Updated
grade
You will work and discuss in pairs for this lab, Before your lab...
BUT you will individually submit a completed 1. Read briefly through…
report. ü Lab 2 (this document)
ADDITIONAL SAFETY NOTES FOR SAFE HANDLING & DISPOSAL ARE EMBEDDED AT THE RELEVANT POINTS IN THE PROCEDURE.
Background
Describing the reactions for the iodine clock and corresponding rate laws
In this experiment, you will study a series of reactions commonly known as an “iodine clock,” named
because we can track the time it takes to produce a certain about of iodine, I2.¹
As you have learned in-class, reactions like this one often happen in several mechanistic steps before
arriving at this overall reaction. Since we do not know the mechanism here, we must determine the
rate law experimentally. To do so, we need to be able to observe or measure how quickly our
reaction is taking place – for example, by measuring how much product is made in a given time, or,
how much time it takes to yield a given amount of product.
Unfortunately, none of the reactants or products has a distinct visual appearance we can track.
Instead, we must track the progress of reaction [1] indirectly – by reacting the products to make new
compounds that we can visualize.
To track the progress of reaction [1], we will rely on two competing reactions where iodine (I2) is a
reactant:
vs.
Once all the S₂O₃²⁻ has been used up, any additional I2
produced by our primary reaction will instead undergo
Reaction [4]. As soon as you see the yellow colour of Timing note
triiodide I3⁻ appear, you know that enough I2 was
produced by our primary reaction to use up any S₂O₃²⁻ The first hint of yellow colour tells us
initially added. In other words, if we know both (i) how when Reaction [4] first begins. If too much
much S₂O₃²⁻ was added and (ii) how much time it took triiodide has formed, your paper will turn
to turn yellow, we can relate these to the rate for brown.3
Reaction 1.
In this lab, we will conduct all of our reactions at a ‘microscale’ or with small amounts of reagents.
Instead of mixing large volumes of our solutions in traditional laboratory glassware like you used in
Lab 1, we will mix small amounts of solution together on a piece of filter paper³ that provides a high
contrast surface to detect the appearance of colour.
Now that we know something about how we can track the rate at which I2 is produced by Reaction
[1], how can we use this information to determine the rate law?
First, let’s focus on the rate you’ll measure, the rate of disappearance or consumption of S₂O₃²⁻. You
can determine the average rate at which it is used up in Reaction 3 in each experiment as follows:
Notice that since the yellow colour only appears once all S₂O₃²⁻ has been used, we know that the final
concentration of S₂O₃²⁻ is zero when you stop your stopwatch. Since you know the initial
concentration of S₂O₃²⁻ at the start of your reaction, these facts combine to help you calculate the
amount of S₂O₃²⁻ used up during that time.
Next, how can you relate the rate of consumption of S₂O₃²⁻ to the rate(s) involved in our primary
reaction? In Reaction [3], we know that the rates at which our two reactants are used up will be
different, since they have different stoichiometric coefficients.
Now, what about relating this back to Reaction [1], which is the focus of our experiment? Since I2 is
produced in Reaction [1] and immediately consumed in the much faster Reaction [3], we can make
the assumption that it is being used up at the same rate that it was produced.
∆[𝐼! ] ∆[𝐼! ]
𝑢𝑠𝑒𝑑 𝑖𝑛 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛 3 ≈ 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑 𝑖𝑛 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛 1
∆𝑡 ∆𝑡
But wait – all rates described so far are average rates! Rate laws, like the one we are trying to
determine, are based on instantaneous rates. Only the initial rate(s) in Reaction [1] can be related to
initial concentrations of our reactants, and used to find the rate law.
• If the reactant concentrations aren’t changing, the average rate(s) over that time interval will
be the same as the instantaneous rate(s) over that same time.
In other words, up until the time the colour appears,
∆[𝐼! ] ∆[𝐼! ]
𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑖𝑛 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛 [1] ≈ 𝑖𝑛𝑠𝑡𝑎𝑛𝑡𝑎𝑛𝑒𝑜𝑢𝑠 𝑖𝑛 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛 [1]
∆𝑡 ∆𝑡
and we can use what we know about related rates again to find the rate of reaction.
Finally, to determine the rate law, you will use a version of the method of initial rates. You will
compare trials or ‘runs’ with different initial concentrations of the reactants from Reaction [1], but
equal amounts of our ‘timer’ chemical, S₂O₃²⁻. By comparing pairs of runs where you varied the
concentration of a single reactant, you can determine how much of an impact each specific reactant
had on the rate you measured.
To simplify your task, we have already determined the order with respect to [H+], or the unknown a in
your rate law [2]. At room temperature and near the concentrations we will be exploring, the rate
law should be 1st order in H⁺ – that means we can re-write the rate law as shown: ²
Procedure
Take notes in the margins during the lab presentation, especially when your TA provides suggestions for
time management.
Part 1: Preparation
2. Divide each circle of filter paper into quarters – since the reactions are microscale, it would be
wasteful to use a full sheet for each run. You will need a total of 21 quarter-sized pieces.
a. Label a 25.00 mL volumetric flask. Deliver one pump (12.5 mL) of stock 0.1 M H₂O₂ (aq)
directly into the flask and add 10 drops of 6 M HCℓ. Dilute to the mark with RO water and
mix well. Pour a portion this solution into a labelled 100 mL beaker so that you can easily
access the solution with an eyedropper.
b. Label a 25.00 mL volumetric flask. Deliver one pump (12.5 mL) of stock 0.2 M KI (aq) directly
into the flask and dilute to the mark with RO water. Mix well. Pour a portion this solution
into a labelled 100 mL beaker so that you can easily access the solution with an eyedropper.
Dilute Stock
Stock Dilute Stock
Solution H₂O₂ (aq) H₂O₂ (aq)
Na₂S₂O₃ (aq) KI (aq) KI (aq)
pre-mixed with H+ pre-mixed with H+
Run 1 1 drop 2 drops ----- ----- 2 drops
Run 2 1 drop ----- 2 drops ----- 2 drops
Run 3 1 drop ----- 2 drops 1 drop -----
Run 4 1 drop ----- 2 drops ----- 1 drop
6. Place a watch glass on top of the white tile from your equipment drawer to give an area of
high visibility for your runs.
7. Place a quarter-piece of filter paper on top of the watch glass. Use a pencil to mark the filter
paper with an ‘x’ to mark the center or target area for adding your reagents (Figure 1A).
1A: Before reaction starts 1B: First hint of brown appears 1C: Too much brown is seen 1D: Extreme example of brown
8. Practice run: Try a practice run to record visual observations in Data Table 2. Your practice run
will follow the amounts for Run 1 in Procedure Table 1 (above).
a. Assign tasks to each partner for each run – one partner will add reactants while the other
operates the stopwatch.
b. When adding each reactant, hold the eyedropper between 0.5-1” above the filter paper.
Too close and you risk contaminating the tip of the dropper by accidentally touching the
surface. Too far and you risk your drops being added off-target.
c. Get ready with the stopwatch. Make sure you have practiced how to start, stop, and reset
before you begin.
d. Add each reactant in order, moving from left to right across the table for Run 1. Use Data
Table 2 on your Lab 5 Worksheet for writing observations.
e. TIMING:
• Start timing at the moment the first drop of H₂O₂ solution is added.
• Stop timing when you see the first hint of yellow-brown colour appear on the filter
paper.
9. Repeat the same steps (a-e) as the Practice Run,
but now focus on recording the time for each Safety note
run and each trial in Data Table 3.
a. Make sure to clean the watch glass Handle filter paper by the edges.
between each trial, including after your
Place used/waste filter paper
practice run.
temporarily into a waste beaker or on
b. Use a new piece of filter paper for each top of a paper towel as you proceed to
trial. the next trial. At the end of the lab, you
will dispose them in the solid chemical
c. You will repeat each run 5 times, before
waste container.
moving onto a different run, for a total of
20 timed trials (not including your practice). Placing filter paper onto the benchtop
d. If you notice visual differences during your can transfer chemicals onto the surface
kinetic runs, note these in Data Table 2. – iodine compounds can stain.
DUE DATE: One week after your lab period, at the regular start time for your lab.
Grade deductions may apply if your submission for this report does not meet all these criteria.
Academic Integrity Note: Remember, even though you collected your data with a partner, your worksheet
should be completed individually. You should use your own data, and you may consult the lab manual, lab
appendices, lecture notes, course textbook, and your TA.
Pre-laboratory preparation
As part of your pre-lab quiz on D2L, you were asked questions about calculations you will use in the lab. Before
you arrive at the lab, use the feedback received on your quiz to layout the sample calculations below so you can
repeat them confidently during the lab period. Show all work for full credit.
You will repeat a similar calculation to determine all initial concentrations in Analysis Table 1 – make sure you
use the actual concentrations from your laboratory room, as recorded in Data Table 1 (not the approximate
concentrations from your procedure).
Data Table 2: Qualitative Observations. Use the space below to record qualitative observations about
the experiment (ex. colour intensity between trials).
Practice Run: Practice Run: Practice Run: Practice Run:
Before you start to add At the first hint of As the reaction After several minutes of
any drops colour on the paper continues reaction continuing
TA initials here
Data Table 3: Iodine Clock Runs – Time required for appearance of initial colour
Run # Trial # Time (s) Average (s)
1
2
Run 1 3
4
5
1
2
Run 2 3
4
5
1
2
Run 3 3
4
5
1
2
Run 4 3
4
5
TA initials here
Data Analysis
Convert the information from Procedure Table 1 and Data Table 1 into initial concentrations that were
actually present on the filter paper.
Analysis Table 1: Calculated initial concentrations and rates for each kinetic run
Keep all calculated values to 3 significant digits in this table – these are intermediates that you’ll use for later
calculations, so rounding them early results in later errors!
REACTION 3 REACTION 1
Run 1
Run 2
Run 4
Sample calculations for initial concentrations were part of your pre-lab work on Page 10 and will be graded there.
Question 1: Sample Calculation – show how you calculated the average rate of consumption of
[S2O32-] for Run 1 in Results Table 1 on the previous page. Report your result with 3
significant digits so that this intermediate value can be used for later calculations.
Question 2: Calculate b, the order of reaction with respect to [I-]. Clearly indicate which runs are
being used in this calculation.
Question 3: Calculate c, the order of reaction with respect to [H2O2]. Clearly indicate which runs are
being used in this calculation.
Question 4: Use your data from Run 1 to calculate k, the rate constant, including units.
Assume that the initial [H+] = 0.00400 M for this run. Recall from the Background that
the reaction is known to be first-order with respect to [H+]. Round your answer to an
appropriate number of significant digits.
Question 5: Summarize your data analysis by stating the equation of the overall rate law for the
reaction studied? Include all values for all orders, and a numerical value of k with units.
Rate =
Question 8: Experimental procedures have assumptions built into their design that can limit the certainty of
our results. We typically refer to these limits of our experiment design as “sources of
uncertainty” or “sources of error.” This experiment, for example, requires each group to reliably
identify the same faint colour change.
Predict how your results would be affected if the timer was stopped only after a darker colour
was seen (i.e. Figure 1C or 1D). Specifically, do you think the rates measured will accurately
represent the initial rate of reaction? Explain why or why not. Use 2-3 sentences.