Experiment 2

Calibration of Volumetric Glassware

For making accurate measurements in analytical procedures, next in importance to
the balance is volumetric equipment which includes glass apparatus used to measure the
volume of a liquid or gas. Some examples are pipets, volumetric flasks and burets.
Volumetric flasks are designed to contain the indicated volume of liquid. The burets and
pipets used in this laboratory are designed to deliver the stated volume of water or dilute
aqueous solution. To indicate this difference, volumetric glassware is usually marked
“TD” meaning to deliver or “TC” meaning to contain. Certain types of pipets, especially
micropipets, are designed to contain a certain volume of liquid and these are marked
“TC”. Despite their simplicity these volumetric glassware are capable of giving very
accurate volume measurements provided they are calibrated and properly used.

There are three general approaches to the calibration of volumetric glassware that
are in wide use.
1. The direct, absolute calibration which is based on the direct mass measurement of
water delivered by a burette or pipet or contained in a volumetric flask and conversion to
volume with the density, at the specified temperature;
2. The indirect, absolute calibration, or calibration by comparison, whereby a calibrated
vessel is used as a reference in the calibration of an unknown vessel, is sometimes used
when many glassware items are to be calibrated; and
3. A relative calibration in which is based on the measured volumetric relationship
between two items of glassware, without knowledge of the absolute volume of either one.

In this experiment, volumetric glassware will be calibrated using the methods of

direct, absolute calibration.

Objectives:

At the end of the experiment, the student should:

 be acquainted with the proper use of volumetric glassware

 be familiar with the methods of direct calibration of volumetric glassware
 apply statistics in treating data
Materials:

Reagents:

Acetone

Equipment and Apparatus:

Volumetric flask Buret

Pipet Thermometer
Erlenmeyer flask Stopcock or cork
Wash bottle Dropper
Beaker Funnel

Procedure:

Table 2-1.Volume occupied by one gram of water at various temperatures, corrected for
buoyancy.

Temperature Volume Temperature Volume

(oC) (mL) (oC) (mL)
18 1.0025 26 1.0043
20 1.0029 27 1.0046
22 1.0033 28 1.0048
24 1.0038 29 1.0051
25 1.0040 30 1.0054

I. Calibration of Volumetric Pipet

1. Place about 200 mL of distilled water in a 250 mL beaker. Allow the temperature
of the water to equilibrate to room temperature.
2. Place a cap on the Erlenmeyer flask and weigh the flask to the nearest mg. Record
this value in your notebook.
3. Record the temperature of the water.
4. Test the pipet to make sure it runs clean by drawing water up above the mark and
allowing it to run back out. Look carefully at the inside wall of the pipet to see if it
is completely clean. The inside should be completely smooth. If there are any
droplets of water on the inside the pipet is dirty and it must be cleaned.
5. Carefully fill the pipet with water up to the graduated mark and deliver the water
to the flask in the appropriate manner. Place the cap on the flask and record the
mass.
6. Repeat steps 3-5 thrice, using the second flask when the first flask becomes full.
 7. Use the difference in mass between each set of two consecutive mass
measurements to determine the mass of water delivered in each trial (thus the
origin of the name “weighing by difference”).
8. Convert the mass of water contained in the flask to true volume applying the
proper correction for the volume of one gram water at various temperature given
in Table 2-1.
9. Calculate the mean volume delivered and the standard deviation.
10. Calculate the percent relative error

II. Calibration of a buret

1. Thoroughly clean a buret (drying is not necessary). Make sure that water drains
well and that the stopcock is lubricated. Fill the buret completely full with
temperature equilibrated distilled water and make sure that air bubbles are not
trapped in the stopcock or tip. Draining water from the buret very slowly, lower
the liquid level until the bottom off the meniscus just rests in the 0.00mL mark.
Touch the tip to the wall of a beaker to remove any adhering drop. Wait 10 min
and recheck the volume. If the stopcock is tight, there should be no preceptible
change in the meniscus.
2. During this time weigh a clean , dry, stoppered 125mL Erlenmeyer flask to the
nearest mg. Record this “initial” weight.
3. Once tightness of the stopcock has been established, slowly transfer (at a rate of
about 10mL/min) approximately 10mL of water to the flask. Touch the tip to the
wall of the flask and stopper it. Wait one minute, then record the apparent volume
delivered from the buret to the second place after the decimal.
4. Refill, using a wash bottle, the buret again to the 0.00mL mark.
5. Weigh the stoppered flask and its contents to the nearest milligram. Determine the
mass of water delivered by difference. Use the data in Table 2-1 to convert this
mass to the true volume delivered. Subtract the apparent volum from the true
volume. This differene is the correction that should be applied to the apparent
volume to give the true volume.
6. Repeat the 10mL calibration at least 2 times. Do not empty and dry the
Erlenmeyer flask between measurements, but make sure that the flask is stoppered
when not receiving liquid.
7. Starting again from the zero mark, repeat the calibration, this time delivering about
20mL to the reciever following the procedure given above. Calibrate the buret
delivering 30, 40, and 50 mL.
8. Prepare a plot of the correction factors (vertical axis) which are to be applied to
convert apparent to true volume versus apparent volume (horizontal axis) of water
delivered. The correction factors which must be applied to any apparent volume
can be read from this graph.
9. Calculate the mean and standard deviation of the correction factor for the burette.
10. Obtain the true volume after correction for 10 mL of water.
Guide Questions

1. Why must oven drying at 80oC of volumetric glassware for more than 3 minutes
not recommended?
- A thin coating of water condensation forms on the surface of glassware
that seems to be “dry.” This water layer must be eliminated when using
chemicals that react with water. You should never expose any volumetric
glassware to heat sources because this will damage the calibration. As a
result, you should never use a drying oven to dry volumetric glassware.
Before using the volumetric glassware, make sure it is properly clean.
Analytical glassware should not be dried in an oven because non-elastic
expansion may occur, throwing the glassware out of calibration.

2. Cite specific techniques for cleaning volumetric glassware.

- Glassware Used for Organic Chemistry
Rinse the glassware with the appropriate solvent. Use deionized water for
water-soluble contents. Use ethanol for ethanol-soluble contents, followed
by rinses in deionized water. Rinse with other solvents as needed,
followed by ethanol, and, finally, deionized water. If the glassware
requires scrubbing, scrub with a brush using hot soapy water, rinse
thoroughly with tap water, followed by rinses with deionized water.

Burets
Wash with hot soapy water, rinse thoroughly with tap water, then rinse
three to four times with deionized water. Be sure the final rinses flow off
of the glass. Burets need to be thoroughly clean to be used for quantitative
labwork.

Pipets and Volumetric Flasks

In some cases, you may need to soak the glassware overnight in soapy
water. Clean pipets and volumetric flasks using warm soapy water. The
glassware may require scrubbing with a brush. Rinse with tap water
followed by three to four rinses with deionized water.

Drying or Not Drying

It is inadvisable to dry glassware with a paper towel or forced air since this
can introduce fibers or impurities that can contaminate the solution.
Normally, you can allow glassware to air dry on the shelf. Otherwise, if
you are adding water to the glassware, it is fine to leave it wet (unless it
will affect the concentration of the final solution.) If the solvent will be
ether, you can rinse the glassware with ethanol or acetone to remove the
water, then rinse with the final solution to remove the alcohol or acetone.
Rinsing with Reagent
If water will affect the concentration of the final solution, triple rinse the
glassware with the solution.

Drying Glassware
If glassware is to be used immediately after washing and must be dry,
rinse it two to three times with acetone. This will remove any water and
will evaporate quickly. While it’s not a great idea to blow air into
glassware to dry it, sometimes you can apply a vacuum to evaporate the
solvent.

Additional Tips
Remove stoppers and stopcocks when they are not in use. Otherwise, they
may “freeze” in place.
You can de-grease ground glass joints by wiping them with a lint-free
towel soaked with ether or acetone. Wear gloves and avoid breathing the
fumes.
The deionized water rinse should form a smooth sheet when poured
through clean glassware. If this sheeting action is not seen, more
aggressive cleaning methods may be needed.