Exp.

2, Fall 2013 17

Experiment 2: Determination of Percent KHP in an Unknown by Titration with
Standard NaOH

Hazardous Waste: No hazardous waste is produced in this experiment.


Prelab Questions
1.) Why do you need to dry the KHP unknown before use?
2.) Equation 1 of the procedure shows you how to calculate the mass of KHP unknown needed for a titration
based on an estimate for %KHP of 40% and the target endpoint volume of NaOH titrant of approximately 35 mL.
In terms of uncertainty, why is an endpoint volume of 9 mL less preferred than an endpoint volume of 35 mL? In
terms of uncertainty, why is an endpoint volume of 55 mL less preferred than a volume of 35 mL?
3.) Lets assume that after the first titration of your KHP unknown, the volume of NaOH titrant is 15 mL and not
35 mL. Does a lower endpoint volume than estimated suggest that the %KHP is less than or greater than 40%?
What change should you make to your procedure for the exact titrations?

Procedure
You will receive your unknown in a vial that has your student number and the experiment number printed on it.
You should record these in your lab notebook. You will need to prepare your unknown for analysis by drying it in
a weighing bottle, just as you did with the pure KHP in the previous experiment. [Hint: label your bottle since
your unknown KHP and the pure KHP from previous experiment may look the same, as well as most organic
substances.]

You will be given 10 g of sample. This should be enough for at least five determinations. You will have enough
for a couple of overtitrations, etc. but not more. If you run out of sample, you may request more, but it will be a
10 point penalty. In the real world, the sample is often a precious commodity that isnt unlimited. Realize that
the number of replicates you are able to perform will depend on the concentration of KHP in your sample. You
will be able to run fewer replicates if you happen to have a sample with a low concentration of KHP. The % KHP
in your sample will be between 20-60%. You will want to set up your analysis (sample size) so that the titration
requires ~35 mL of titrant. This will of course be dependent on the particular concentration of your sample, so
you will want to estimate an approximate sample size for the first titration. First, assume your sample is
somewhere in the middle of the range (i.e. 40%). Using the standardized concentration of your base, calculate the
necessary sample mass that will require 35 mL of titrant (eqs 1-2).

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) (

) (1)



(2)

You can then perform a single titration on a single sample to determine the approximate concentration of your
unknown. (Use proper technique, such as weighing by difference) If you happen to hit the end point very
precisely, you can use the answer in your final statistical analysis. You shouldnt, however, waste much time on
this first titration as the main point is simply to get the approximate concentration in order to set up the sample
size for the rest of the titrations.

Once you know the approximate concentration of your sample, you can calculate the mass of sample required to
titrate to endpoint with 35 mL of your base. It is absolutely critical here that you properly weigh by difference
using your weighing bottle and that you accurately record to the full precision of the balance the mass of each
sample. These should all be within 0.1 g of your target mass. Since you are unlikely to have each sample with
Exp. 2, Fall 2013 18
exactly the same mass, you can use the ratio (volume of base / mass of sample) to determine the approximate
volume that will be required for each replicate titration.

You should accurately titrate at least three samples. If you have remaining sample and adequate time, additional
replicates can only help your determination (if done properly). [Hint: you can rapidly titrate to within a milliliter
or so of the expected endpoint and then do a careful drop-wise and partial drop titration. In other words, use your
time where it counts and be quick where it doesnt.]

Calculate the percent KHP for each of your replicate samples. If you have a data point that is not known to
contain a gross error, but seems very much out of line with the other data, you can consider statistical justification
of omitting the data with the Grubbs test (section 4-6 of the Harris text). This should be done with extreme
caution, especially on very small data sets. It is very possible the datum that looks out of line is actually balancing
an opposite bias in the other data. Using at least three replicate values, calculate the mean and standard deviation
for the unknown.

Data Reporting

Using the standard deviation you calculated, report you average %KHP with its 95% confidence interval (see
table 4-6) in the Harris text.

Once you are satisfied with your data and your calculations, you will report your final answer for the
determination as the average% KHP confidence interval along with your student number. Because confidence
interval depends on the number of replicates (n) and the %confidence level used, you must also always report
these values. Then, draw a box around your answer so your instructor will know what to grade. Use the format
shown on page 4 in the front materials of the lab manual, and an example is below. Make sure your table of
contents is up to date, and then turn in your notebook for grading.

Example:

Experiment 2
Student # 1
%KHP = (42.3 0.5)%
n = 3, 95%