1
UNIVERSITY OF MINES AND TECHNOLOGY (UMaT),
TARKWA
DEPARTMENT OF CHEMICAL AND PETROCHEMICAL
ENGINEERING
EXPERIMENT 1
A REPORT ON THE CALIBRATION OF PIPETTE
FEBRUARY 1, 2024
BY
ANIM POKUAH KAKARI WILHELMINA
(SPE.41.014.022.22)
GROUP 4
CLASS: RP 2
COURSE NAME: CHEMISTRY LABORATORY PRACTICES (RP 273)
COURSE LECTURER: DR. JOHANNES AMI
2
ABSTRACT…………………………………………………….. 3
INTRODUCTION………………………………………………. 4
MATERIALS AND PROCEDURE……………………………. 5-6
RESULTS…………………………………………………………7-8
CALCULATIONS……………………………………………….. 9-10
DISCUSSIONS……………………………………………………. 11-12
SOURCES OF ERROR………………………………………13
CONCLUSION……………………………………………………14
ANSWERS TO POST LAB QUESTIONS………………………15-16
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ABSTRACT
This laboratory experiment focused on the calibration of a pipette to enhance
precision and accuracy in volume measurements. The objective was to ensure reliable
and consistent performance of the pipettes, crucial in various chemical applications.
The calibration process involved measuring the delivered volumes of distilled water
using a gavimetric method. The results indicated minor deviations from the target
volumes, suggesting the need for re calibration and meticulous handling. This study
emphasizes the importance of of regularly calibrating pipettes to maintain their
efficacy and reliability in laboratory procedures, ultimately contributing to the overall
accuracy of experimental outcomes.
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INTRODUCTION
Calibration is defined as the act of making sure that a scientific process or
instrument will produce results which are accurate. In more complex terms,
calibration is the act which determines the functional relationship between measured
values and analytical quantities. In many laboratory experiment, small amounts of
reagents must be dispensed not only very accurately but with a great deal of precision.
However, one of those glassware is the pipette. A pipette is a small piece of
laboratory apparatus used for measuring and dispensing small volumes of liquids.
Hence, Pipette Calibration is the method of designing or adapting pipettes in such a
way that they provide results for samples within an acceptable range. Accuracy is the
closeness degree of measurement with the actual value. Precision, on the other hand is
the closeness of two or more measurements to each other.
The standard Deviation can also be used to get the accuracy of measurements.
If the high proportion of data lies near the value of mean. It has lower standard
deviation. Lower standard deviation indicates lower accuracy of measurements. There
is a need for calibration as it leads to maximized productivity, optimization of results,
the product can be accepted everywhere, ensures safety of employees and consumers,
reducing cost and time, maintaining the quality and ensuring the effectiveness of the
result of all experiments.
The purpose of this experiment was to calibrate the pipette and use it to
measure the density of an unknown liquid. Pipettes come in several designs for
various purposes with differing levels of accuracy and precision. The volumetric,
measuring and mechanical micro pipettes are the three most common types found in a
laboratory. The pipette can be used to measure the density of an unknown liquid using
the equation, D=M/V. However, beforehand, the volume of the pipette must be
identified first by getting the mass of the distilled water and the known density of
water at 25 Celsius degrees. The density of distilled water at 25 Celsius degrees is
0.9971g/cm^3. By deriving the equation D to V, the volume of the pipette can be
found after taking the average.
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MATERIALS AND PROCEDURE
Materials
The materials used in this experiment were;
Pipette,analytical balance,small beaker,pipette bulb,tissue paper and unknown liquid.
Procedure
Part 1
Calibration of the pipette was done in this part.
This experiment presents the detailed procedure in calibrating a pipette to determine
the volume of a solution of known density, weigh the the amount transferred, and
determine if the volume corresponds to the indicated volume.
Distilled water was obtained with its temperature recorded with the liquid in class
thermometer.This procedure is done as a result of temperature being a factor affecting
density. With the use of an analytical balance, a clean and dry 50mL beaker was
weighed to the nearest ±1mg. The value was then recorded as the mass of the
container. A pipette was then cleaned so that no water droplets of distilled water was
left on its inside surface. It was then filled with water with the help of the pipette bulb.
The outside of the pipette was then cleaned thoroughly with a tissue paper. The
meniscus was then adjusted to reach the marked line of the pipette. The content was
dispensed into the beaker till the last drop using the force from the pipette bulb. This
was then weighed using the same analytical balance. This step was repeated until we
had results for 3 trials. The mass of the water was calculated by using the formula:
mass of empty container(g)- mass of container with water(g) and the value was
recorded. Therefore with the mass and density of the sample now at hand, the volume
of the sample and that of the pipette was obtained. This was done by calculating the
volume using the equation, V = M/D where M is the mass of the water and D is the
density of water at 25 Celsius degrees. After getting the volumes for all the trials, the
average was then taken with the answer being the volume of the pipette.
Part 2
The determination of the density of the unknown liquid was contained in this part. A
clean and dry 50mL beaker was weighed using the analytical balance and the value
recorded. Several portions of the unknown(oil) was drawn into the pipette to the
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marked line. It was then transferred to the prerecorded beaker and the content together
with the beaker was weighed and their mass recorded. The mass of the oil was then
found using the relation as used earlier for the water.
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RESULTS
Table 1.1( table of results for first experiment)
Calibration of Pipette
Trial 1 Trial 2 Trial 3
Mass of 51.798 50.203 49.451
container(g)
Mass of container 61.843 60.246 59.489
and water(g)
Mass of water(g) 10.045 10.043 10.038
Volume of 10.074 10.072 10.067
water(cm3)
Temperature of 25.000 25.000 25.000
water (℃)
Average volume of 10.071
pipette(cm3)
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Table 1.2( Table of recorded values of 2nd experiment)
Trial 1
Mass of empty container(g) 52.351
Mass of container and sample(g) 60.492
Mass of sample(g) 8.141
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SAMPLE CALCULATIONS
For Trial One;
Mass of container= 51.798g
Mass of container with water= 61.843g
Mass of water =61.843-51.798=10.045g
Density of water at 25℃= 0.9971g/cm3
����
Density = ������
����
Hence; Actual volume of pipette=
�������
10.045
Actual volume= 0.9971 = 10.074cm3
For Trial Two;
Mass of container= 50.203g
Mass of container with water= 60.246g
Mass of water=60.246-50.203= 10.043g
����
Actual volume of pipette= �������
10.043
Actual volume= 0.9971 = 10.072cm3
For Trial Three;
Mass of container = 49.451g
Mass of container with water= 59.489g
Mass of water= 59.489-49.451= 10.038g
����
Actual volume of pipette=�������
10.038
Actual volume= 0.9971 = 10.067cm3
10.074+10.072+10.067
Average Volume of Pipette = 3
Average volume= 10.071cm3
Therefore, the average volume of the pipette is 10.071cm3
10.071−10.074) ²+(10.071−10.072)²+(10.071−10.067)²
Standard deviation= 3−1
Standard deviation= 0.00361
10
�
Relative standard deviation,SR = � x 100
0.00361
= 10.071 x100
=0.0358%
�
Relative standard deviation in ppt =�x1000ppt
0.00361
= 10.071 x 1000ppt
= 0.3555ppt
Obtained result
10.071−10
Relative error percentage= 10
x100%
Relative error percentage= 0.71%
FOR OIL
Mass of oil= 60.492-52.351
Mass of oil= 8.141g
���� �� ���
Density of sample(oil)= ������ ������ �� �������
8.141
ρ=
10.071
ρ =0.808g/cm3
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DISCUSSIONS
The calibration data for the 10mL pipette is presented in Table 1.1. The
average volume obtained for the pipette is 10.071cm3. The standard deviation for
the calibration is 0.00361. The calibration of the pipette was conducted to ensure
accurate and precise volume measurements during experimental procedures. The
comparison of measured volumes with the expected values showed a generally good
agreement, with minor discrepancies observed in some measurements. The mean
volume across all trials was found to be 10.071cm3, with a standard deviation
deviation of 0.00361, indicating consistent performance of the pipette within the
specific range. However, further examination of the data revealed variability in the
replicate measurements, as evidenced by the calculated relative standard
deviation(RSD) of 0.03%. The calibration process involved measuring the mass of
water and using the density of water at a specific temperature to convert mass into
volume.Water,with a density of 1g/cm3 is the most affordable and common type of
liquid that can be used in calibration of pipette. At higher temperature values there
is going to be expansion of the water increasing the volume but the mass remains
the same. This is due to the inter-molecular structure of water which shows a
variation of it density with respect to temperature changes. This results in decreased
density of the water sample with respect to temperature increment. The meniscus of
the water was used to indicate the mark on the pipette.
SOURCES OF ERROR
However, it was important to note that there were some sources of errors that may
have contributed to variations in the measured volumes. One potential source of
error was human error, such as variations in techniques when operating the pipette
or reading the meniscus. Another potential source of error was environmental
factors, which could have affected the viscosity of the liquid being pipetted and
thereby impacting the accuracy of volume measurement. In addition, the calibration
process itself may have introduced some degree of error as it relied on the accuracy
of the standard solutions used for comparison. To improve the accuracy of
calibration, it may be beneficial to use multiple standard solutions spanning a range
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of volumes and concentrations. Parallax error occurred due to the eyes being above
or below the meniscus of the pipette. Another source of error was that the
remaining droplets of water was left in the measuring instruments after the previous
measurements. Last but not least, the error occurred due to incorrect technique
when instruments were being used. For example, the remaining water was left in the
tip of the pipette due to wrong technique of using this instrument.
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CONCLUSION
From this experiment, it can be concluded that calibration is vital for the purpose
of maintaining the accuracy of instruments.The result of this experiment shows that
the gavimetric method is a reliable method for calibrating pipettes. The result of the
experiment also show that the pipette used in this experiment was accurate to
within ±0.015cm3. Overall, the calibration result provide confidence in the reliability
of the pipette for use in laboratory experiment, while also highlighting the
importance of ongoing quality assurance measures to maintain accuracy and
precision in volume measurement
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REFERENCES
1. Rani, Seema; Khan, Tasneem K. H.; Mote, Sanjay P.; Gehlot, Praveen Singh
(2023). An Introduction To Analytical Chemistry. Academic Guru Publishing House.
p. 158. ISBN 9788119338009. "ANSI/NCSL Z540.3-2006 (R2013)". The National
Conference of Standards Laboratories (NCSL) International. Archived from the
original on 2014-11-20. Retrieved 28 November 2014.. ^ "Calibration Systems
Requirements (Military Standard)" (PDF). Washington, DC: U.S. Department of
Defense. 1 August 1998. Archived from the original (PDF) on 2005-10-30.
Retrieved 28 November 2014.
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ANSWERS TO POST LAB QUESTIONS
Q1.
Set A Set B Set C Set D
325mg 300mg 400mg 250mg
325mg 325mg 400mg 280mg
325mg 350mg 400mg 350mg
1. a. Set A is said to be precise and accurate. The true value for the aspirin content is
325mg and in set A, all the samples are the same as the true value. It is also precise
because upon their reproducibilty, they are still the same hence, the closeness(same)
to each other.
b. Set B is precise but not accurate. This is because the series of measured values
are close to each other but not the same.
c. Set C is said to be not precise but accurate because the measurement vary
widely but are close to the true value .
d. Set D is said to be neither precise nor accurate because for the values above,
their differences are huge making them not precise nor accurate as they are far from
the true value also.
Q2) Using a dirty pipette with residual drops of liquid can lead to inaccurate volume
measurements. The remaining drops can alter the volume of liquid dispensed with
each use, causing the measured volume to be consistently higher then the actual
volume. This would result in an overestimation of the volume of the pipette. To
ensure accurate measurements, it’s essential to properly clean and dry the pipette
between uses to eliminate any residual liquid.
Q3) If the balance consistently gives masses that are 20mg higher than the true
masses, it would lead to systematic errors in the experiment. All measurements taken
using the balance would be consistently higher than the actual values. This could
affect the accuracy of the experiment’s results, causing them to be consistently
overestimated by 20mg.
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Q4) Ensure the pipette is cleaned is clean and free from any residual liquid before
each use. Use proper pipetting techniques to minimize errors. Calibrate the pipette
regularly to ensure accuracy. Use a balance with a small margin of error or one that
has been properly calibrated. Repeat the measurements multiple times and calculate
the average to reduce random errors. The level of the eye should be perpendicular to
the line marked. This is going to reduce to make proper viewing of the meniscus at
the right point.