Experiment 1 Calibration of Glass wares

In this laboratory exercise, we will calibrate the two types of glassware typically used by an analytical
chemist; a volumetric flask and a burette. Over the course of this semester, we will use these tools
extensively when performing Gravimetric and Titrimetric Analyses. To avoid introducing Systematic
Errors into our measurements, each of these instruments must be properly calibrated. And, to reduce
the Random Errors inherent when using these instruments, their proper use must be thoroughly
understood. The quality of the measurements obtained from these tools depends heavily on the care
taken in calibrating and in using each instrument.

DEFINITIONS:

 Accuracy is the closeness of agreement between a measured value and the true value.

 Precision is the closeness of agreement between independent measurements of a quantity

under the same conditions.

 Uncertainty is the component of a reported value that characterizes the range of values within
which the true value is asserted to lie.

 Error is the difference between a measurement and the true value of the object being
measured. Error does not include mistakes.

 Deviation = abs (mean -value)

 Av Dev = Deviation/N;
 % error = (abs (true value-experimental value))/true value *100

Types of Error
The error of an observation is the difference between the observation and the actual or true value of the
quantity observed.
Errors are often classified into two types:
Random:
Random errors vary in a completely non-reproducible way from measurement to measurement. but can
be treated statistically, and so relate the precision of a calculated result to the precision with of the
measurements taken.
Systematic:
Systematic errors may be caused by problems in either the equipment, the observer, or the use of the
equipment. Systematic errors can result in high precision, but poor accuracy. They are difficult to
discover. Examples:
♦ A student may overshoot the endpoint of a titration over and over again.
♦ A balance may always read 0.001 g more because it was zeroed incorrectly. .
calibration of Volumetric Flasks

The Volumetric Flask is used to prepare Standard Solutions or in diluting a

sample. Most of these flasks are calibrated To-Contain (TC) a given volume of
liquid.

1. Clean three different sizes volumetric flasks 10 mL, 25 mL, & 50 mL. Dry
and record the mass of empty flask
2. Calibrate by filling each to the mark and weigh.
3. Perform 5 trials for each flask.
4. Calculate mass of water (subtract mass of filled flask – mass of dry flask)
5. This mass is then converted to the desired volume using the tabulated
density of Water:
6. Use the experimental water volumes (= mass of water / density at 22 0C))
to calculate deviation from mean, average deviation, and average %error
for each pipet.
7. Plot their average deviations and %errors vs. volume of the 3 flasks
8. Discuss your results.

Calibration of a Burette

Sources of error in burette use:

 a dirty burette that does not drain evenly.
 an air bubble in the stopcock of burette tip
 parallax errors
 delivering the liquid too rapidly so that liquid on the side does
not have time to drain.
 not reading the burette properly
Use of a Burette
1. Add 5 to 10 mL of the titrant, rotating to wet the interior
completely, then drain. Repeat.
2. Make sure the burette is clamped in a perfectly vertical position.
3. Fill the burette to above the zero mark and drain some solution to free the burette tip of
bubbles.
4. Drain the solution to the zero mark and record the starting reading after 1 min. You
don’t have to be at precisely zero, but you do have to precisely record the initial
reading.
 Use your cleaned 50mL burette. Fill the burette with water. Make sure the tip is free of bubbles. Drain
into a waste beaker until it is at, or just below, the zero mark. Allow 10-20 seconds for drainage. Make
an initial reading to a precision of at least 0.01 ml.

Weigh a receiving container (50 mL beaker) on the Analytical Balance; cover

with Aluminum foil. Drain 10 mL of water from the burette into the beaker.
Weigh the water after transfer.

Repeat the procedure at increments of 10.00 mL until you have made 5

measurements. You should have delivered ~ 50 mL from your burette at this
point. This mass is then converted to the desired volume using the tabulated
density of Water.

Note: for each increment of 10 mL make sure you are not losing any drop of
water in between the measurements. And if it is slightly lower or higher
than 10 mL, record the exact volume delivered and use it in the calculations.

 Perform 5 trials for each volume.

 Use the experimental water volumes (= mass of water / density at 22
0
C) to calculate deviation from mean, average deviation, and average
%error of all the measurements made.
 Plot their average deviations and %errors vs. volume of water,
delivered from burette.

As was done for volumetric flask.

Deviation = abs (mean -value)

Av Dev = Deviation/N;

Plot average deviation vs. volume

For each data point: % error = (abs (true value-experimental value))/true value *100

Calculate mean % error vs volume.

Calculations and report:

 Follow the guidelines for lab report write the report.
 Provide one written example for one set of data calculation.
 However, all calculations must be performed using excel.
 Turn-in hard copy and an electronic copy of your report via blackboard along with the excel file.

Post lab questions:

1) What is the purpose of calibration?

2) Why do you have to use the correct volume instead of the mass of water?
3) What is the difference between average deviation and percent error?

4) How do you expect the shape of each graph? Why?

Appendix - Density of Water

T (oC) Density (g/mL)

10 0.9997026

11 0.9996084

12 0.9995004

13 0.9993801

14 0.9992474

15 0.9991026

16 0.9989460

17 0.9987779

18 0.9985986

19 0.9984082

20 0.9982071

21 0.9979955

22 0.9977735

23 0.9975415

24 0.9972995

25 0.9970479

26 0.9967867