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AnaChem-Lab-4

The document outlines a laboratory exercise focused on calibrating a pipette, emphasizing the importance of accurate measurement and proper technique. It details the procedure for calibration, including cleaning the pipette, measuring mass, and correcting for buoyancy. The exercise aims to ensure reproducibility and precision in volumetric measurements using a pipette.

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IvyCamille Omila Belano
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4 views

AnaChem-Lab-4

The document outlines a laboratory exercise focused on calibrating a pipette, emphasizing the importance of accurate measurement and proper technique. It details the procedure for calibration, including cleaning the pipette, measuring mass, and correcting for buoyancy. The exercise aims to ensure reproducibility and precision in volumetric measurements using a pipette.

Uploaded by

IvyCamille Omila Belano
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Analytical Chemistry 1 Laboratory

Exercise No. 4
CALIBRATING A PIPETTE

OBJECTIVES

1. To know the importance of calibrating a pipette


2. To learn the proper technique in calibrating a pipette

BACKGROUND

Volumetric glassware is calibrated by measuring the mass of liquid (usually


distilled water) of known density and temperature that is contained in (or
delivered by) the volumetric ware. In carrying out calibration, a buoyancy
correction must be made since the density of water is quite different from that of
the weights.

All glassware should be freed of water breaks before being calibrated. When a
pipette, burette, or another piece of volumetric glassware is cleaned properly, no
droplets of reagent remain on the internal surfaces when they are drained. This
is very important for accurate and reproducible results. If the reagent adheres to
the inside of a pipette, the nominal volume of the pipette cannot be delivered.

The water used for calibration should be in thermal equilibrium with its
surroundings. The condition is best achieved by drawing the water in advance,
noting its temperature at frequent intervals and waiting until no further changes
occur.

The calibration of a volumetric pipette should start by determining the mass of


an empty stoppered receiver to the nearest milligram. The temperature-
equilibrated water will then be transferred to the receiver using the pipette. The
mass of water delivered will then be calculated from the difference of the mass
of the receiver with water and the mass of the empty receiver. The volume of
water delivered will be computed by a buoyancy correction factor.

REAGENTS

Distilled water

School of Chemical Engineering and Chemistry 12


Mapua Institute of Technology
Analytical Chemistry 1 Laboratory

APPARATUS/GLASSWARE

10-mL pipette
50-mL Erlenmeyer flask
400-mL beaker
Analytical balance
Cork stopper
Suction bulb
Thermometer

PROCEDURE

1. Clean a 10-mL pipette. When a pipette, burette, or another piece of


volumetric glassware is cleaned properly, no droplets of reagent remain
on the internal surfaces when they are drained. This is very important for
accurate and reproducible results. If the reagent adheres to the inside of a
pipette, the nominal volume of the pipette cannot be delivered.

NOTE: In cleaning a pipette or any other glassware with alcoholic KOH,


use a bottle of cleaning solution and rinse it off thoroughly before
returning the pipette to the shelf. Do not put the bottle of cleaning
solution directly on a bench top; it may ruin the surface. The solution is
very corrosive. If your fingers feel slippery after using the solution, or if
some parts of your body develop an itch, wash the area thoroughly with
water.

2. Obtain a 400-mL beaker of distilled water equilibrated to room


temperature.
3. Determine the mass of the flask and the stopper and record it to the
nearest 0.1 mg.

NOTE: Do not touch the flask after the weighing. Use tongs or a folded
strip of waxed paper to manipulate the flask.

4. Measure and record the temperature of the water.


5. Pipette 5 mL of distilled water to the flask. Stopper the flask, determine
the mass of the flask and the water and record the mass.
6. In the same way, add a second 5 mL of water to the flask; remove the
stopper just before the adding. Replace the stopper, and once again
determine and record the mass of the flask and the water.

NOTE: Following each trial, determine the mass of the water added to the
flask.

School of Chemical Engineering and Chemistry 13


Mapua Institute of Technology
Analytical Chemistry 1 Laboratory

7. Repeat this process until you have determined four consecutive masses of
water that agree within a range 0.02 g.

NOTE: If the determinations of masses of water delivered by the pipette


do not agree within this range, the pipetting technique may be wrong.
Request your instructor for assistance in finding the source of the error,
and then repeat the experiment until you are able to deliver four
consecutive volumes of water with the precision cited.

8. Correct the mass for buoyancy and calculate the volume of the pipette in
milliliters.
9. Report the mean, the standard deviation, and the relative standard
deviation of the volume of the pipette. Calculate and report the 95%
confidence interval for the volume of the pipette.

School of Chemical Engineering and Chemistry 14


Mapua Institute of Technology

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