KUMASI TECHNICL UNIVERSITY

DEPARTMENT OF CHEMICAL ENGINEERING

INORGANIC AND ANALYTICAL CHEMISTRY

TITTLE OF EXPERIMENT;PIPETTE CALIBRATION

LECTURER;REV. JOHANNES AMI

CALIBRATION OF PIPETTE

INTRODUCTION;

Calibration is an evalution among measurement. Measurement technology and

metrology is the comparison of measurement values delivered by device under test
with those of a calibration standard of known accuracy such a standard could be
another measurement device of known accuracy,a device generating the quantity to be
measured such as a voltage ,sound tone,or a physical artefact ,such as a meter ruler.

The outcome of the comparison can result in no significant error being noted on the
device under test,a significant error being noted but no adjustment made,or an
adjustment made to correct the error to an acceptable level,strictly speaking ,the term
calibration means just the act of comparison ,and does not include any subsequent
adjustment. The calibration standard is normally treceable to a national standard held
by a National Metrological Institute.

One of known size or correctness made or arranged along with on particular device
and another measurement made in as similar way as possible with a second gadget.This
experiment introduces us to pipette calibration.

Pipette calibration is predominantly undertaken by gravimetric analysis.The

gravimetric analysis entails dispensing samples of distilled water into a receiving
vessel in a precision analytical balance.

The density of water is a known constant, the temperature, barometer pressure and
humidity are recorded(Z-factor used in the final mass calculation)and kept within
certain limits and thus the mass of the dispensed sample provides an accurate indication
of the volume dispensed.

A pipette is a laboratory tool to transport small amounts of measured liquid accurately

by aspiration and dispensing the sample .Pipette is calibrated when the expected
volume with the actual volume delivered by a pipette are determined together with the
associated measurement uncertainty by an accredited institution.Purpose of calibrating
is to prove if the pipette is still within its manufacture specification to deliver accurate
results.

Pipette out of tolerance can be adjusted or re-calibrated.Pipettes can typically used in

chemistry ,biology,clinical and medical areas, where liquid samples are taken and must
be transported often in small and accurate quantities for further dilutions,research and
analysis work.

Pipette calibration shows the difference between expected and actual volume,which
shall be within a given tolerance.If it is outside tolerance it can produce falsch dilutions
and in the end even wrong analytical results.

Reasons for calibration;

 A new instrument.

 After an instrument has been required or modified.

 When a specified time period has elapsed.

 When a specified usage (operating hours)has elapsed.

After an event ,for example ,after an instrument has been exposed to to a

shock,vibration ,or physical damage ,which might potentially have compromised the
integrity of its calibration or sudden changes in weather.

In general use,calibration is often regarded as including the process of adjusting the

output or indication on a measurement instrument to agree with value of the applied
standard ,within a specified accuracy. For example, a thermometer could be calibrated
so the error of induction or the correction is determined, and adjusted (eg.via
calibration constant so that it shows the true temperature in celsius at specific points
on the scale. This is the perception of the instruments end user.
However very few instruments can be adjusted to exactly match the standards they are
compared to. For the vast majority of calibration, the calibration process is actually the
comparison of an unknown to a known and recording the results.

Therefore;

Accuracy is defined as nearness to the true value and precision is a measure of the
reproducibility of a result.

The experiment was to investigate the precision and accuracy of a pipette by making
accurate of a pipette by making accurate determinations of the mass of the water it
delivers in repeated operations.

APPARATUS;

Pipette

Thermometer

Beaker

Analytical balance

Unknown solution

Water
PROCEDURE;

Firstly the pipette and beaker were cleaned, afterwards the mass of the beaker was
obtained by weighing it with an analytical balance as accurately as possible and was
then recorded.

The pipette was carefully filled with water, the water was adjusted to the line and was
then transferred to the already weighed beaker with giving it enough time for the
residue at the tip to drop.

The container together with the water in was then weighed and the value was recorded.

Temperature of water was then recorded using the thermometer.

This procedure was repeated three times.

And in retrospect this same procedure was used for unknown solution to get the
mass,volume etc..

PRECAUTION;

1. Gloves were worn throughout.

2. During pipetting,the pipette bulb was used.

3. The balance was treated with care since its a delicate instrument.
RESULTS AND DISCUSSION;

Considering the value for the masses taken, there was an error and this could be as a
result of trying to rinse and clean the weighing bottle and some traces of water might
have been left on the weighing bottle which might have increased the mass of the water
in the weighing bottle.And failure to allow the pipette enough time to drain.Though
the values may differ from the expected value but calibration helps to determine the
actual unit of a substance.

DATA AND CALCULATION;

EXPRIMENT TABLE 1-1;

TRIAL 1 TRIAL 2 TRIAL 3

Mass of container 57.540g 57.665g 57.640g

and water.

Mass of empty 32.731g 32.719g 32.718g

container.

Mass of water. 24.809g 24.946g 24.922g

Temperature of 32oC 32oC 32oC

water.

Volume of water 24.954ml 25.092ml 25.067ml

True volume of 24.954ml 25.092ml 25.067ml

pipette.

24.809 g  24.946 g  24.922 g

Average mass of water =
3

=24.892g

24.954ml  25.092ml  25.067ml

Average value for volume of pipette=
3

=25.037ml

How to calculate for volume of water;

mass
Density=
volume

Temperature varies with density hence

Temperature reading=32oC and density =0.9942g/ml

Then for trial 1;

24.809
0.9942=
V
V=24.954ml

For trial 2;

24.946
0.9942=
V

V=25.092ml

For trial 3;

24.922
0.9942=
V

V =25.067ml

For unknown solution;

Mass of empty container 32.747g

Mass of container and unknown solution 58.481g

Temperature of unknown solution 32℃

Volume of unknown solution 25.884ml

Mass of unknown solution 25.734g

True titre volume of pipette 25.884ml

X Actual mean X-actual mean (X-actual mean)2

24.954ml 25.037ml -0.083 6.889×10-3

25.092ml 25.037ml 0.055 3.025×10-3

25.067ml 25.037ml 0.03 9×10-4

  ( x  Am)
2

Standard deviation=√ N 1

=√
 (0.010814)
2

=0.074

calculatedvalue  actualvalue
Percentage relative error=
actualvalue

25.037  10
= *100
10

=15.037％

Relative standard deviation=

0.074
= *1000 pt
24.892

=2.973％

REFERENCE;

Crouch,Stanley&Skoog,Douglas A(2007).Principles of instrumental Analysis .Pacific

Grove:Brooks Cole