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Principles of Analytical Chemistry, Laboratory
Abstract
Calibration of glassware is essential to ensure accurate results in all laboratory settings. The major goals of this
experiment are to understand the effects of temperature and buoyancy on weighing as well as the correct methods for calibrating
volumetric glassware and the significance of accurate volume reading in analysis. The experiment examines the accuracy with
which two different volumetric glassware types measure liquid quantities in quantitative laboratory work. To ensure that the
glassware is free of any particles or dirt that might affect the measurement's precision, the experiment starts by thoroughly
washing it in a warm detergent solution. In order to achieve the best results, thorough preparation of the solution and the glassware
is done using techniques including almost horizontal buret tilting to force air bubbles out of the glassware and avoiding touching
the glassware with bare hands. Carefully pour 10 mL of water into the flask from the buret, then cover it to stop evaporation.
Repeat the process, adding a following 10-mL increment to the same flask, until a total of 50 mL has been delivered. When
calculating real mass (MT), make sure to always check the significant figures. The calculated Cumulative Correction Factor
(CCF) must then fall within the buret's tolerance range. This experiment's inaccuracy could be caused by improper usage of
volumetric glassware. Aspirator should first be used to fill the 10-mL pipet. A 50 mL Erlenmeyer flask needs to be filled with
water once it has been weighed and recorded. Run three trials for this calibration.
Keywords: calibration, glassware, inaccuracy, measurement, buret, pipet
Calibrating volumetric glassware is a critical step in
Introduction
ensuring accurate measurements in a laboratory setting.
According to the definition given in the
However, there can be gaps or challenges in the calibration
International Vocabulary of Metrology (JCGM 200: 2012,
process that need to be addressed to maintain precision and
Definition 2.39), calibration establishes a relation between
reliability in your experiments. Here are some common gaps
the quantity value provided by a measurement standard and
or issues that can arise when calibrating volumetric
the corresponding indication provided by a measuring
glassware. Human error is a significant source of calibration
instrument or system. Calibration also requires
gaps. This can include misreading the meniscus and not
determination of the uncertainties associated with the
properly cleaning or drying the glassware. Variations in
measurements performed. Calibration of instruments and
temperature, pressure, and humidity can affect the accuracy
processes is absolutely essential for correct operations and
of volumetric glassware. The instruments used for
for checking their performances against known standards.
calibration, such as balances and thermometers, can
This provides consistency in readings and reduces errors,
introduce errors if they are not calibrated or maintained
thus validating the measurements universally.
regularly. Volumetric glassware can degrade over time due
The specific objectives of this experiment are to to chemical exposure, physical damage, or regular use.
learn the proper techniques for calibrating volumetric
This experiment aims to ensure accuracy and
glassware, learn the importance of accurate volume reading
reliability in volume measurements, to determine how
in analysis, and understand the effect of temperature and
precise the glassware is at measuring volume, aims to assess
buoyancy in weighing. We intend to account for temperature
and improve the precision of the glassware by measuring its
variations as glassware calibration can be temperature
repeatability and the consistency of its measurements over
sensitive, measure the repeatability and consistency of
time, it also aims to use the proper technique in calibrating
volume measurements to determine the reliability of the
volumetric glassware, and ensure that all measuring
glassware, and calculate the uncertainty associated with
equipment is properly calibrated.
volume measurements to provide a measure of the reliability
of the calibrated glassware. It is crucial to calibrate
Experimental
volumetric glassware since it enables you to assess its
This experiment aims to calibrate the glassware to
effectiveness and quality. Maintaining the quality of
increase precision and reduce systematic error. One of the
laboratory results and reducing potential errors need
most efficient ways to do this is through glassware
accurate calibration of the glassware.
1
Cagampang, N.I.S. CHY 46.1
calibration. The procedures that follow show the many
evaluations that were made throughout the experiment.
Materials
Analytical balance was used to accurately measure
the mass of water being dispensed from the buret and the
pipet. It served as a check to make sure the right amount of
liquid was being given. During calibration, the buret and
pipet were filled with distilled water. Using distilled water
makes it easier to avoid impurities that can impact the
calibration's accuracy. The amount of distilled water
dispersed from the buret and pipet was measured in a 50-mL
Erlenmeyer flask with a stopper. This aids in determining
the device's accuracy. For calibration, a buret holder fixed
on an iron stand with a 50-mL buret and a 10-mL pipet were
utilized.
Methodology
A. Schematic Diagram of 50mL Buret Calibration
Figure 1. Buret reading (bottom of meniscus)
[4]The weighted flask was gently filled with around
10mL of water, which was then poured in and covered to
prevent additional evaporation. In order to read the final
volume (Vf), the flask was set for 30 seconds so that the
liquid covering on the walls would disappear. The flask with
a stopper was weighed again to check the final mass (Mf).
The appropriate row of the 10mL volume was then recorded
with the Vf and Mf. [5]Using the same procedures as in step
4, an additional 10mL of water (for a total of 20mL) was
added to the weighted flask. Mf and Vf were recorded in
correlation to the 20mL volume increment. Keep adding
10mL of water to the same flask up until 50mL of water and
record the results. [6]After the first trial, the buret was filled
with water. A total of three trials were conducted by
repeating procedures 3-5 using another dry flask with a
stopper. [7]The first 6 columns of table 1 were completed.
For specific volume increment (V) findings, Vd or Md were
calculated by subtraction of Vf and Mf right above it. [8]The
true mass (Mt) was determined by adjusting the delivered
mass (MD) to take into account the buoyancy of water in air.
[9]Mt was divided by the density of water which resulted to
the calculation of true volume Vt and correction factor was
calculated. A plot in Excel Sheet was prepared.
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Cagampang, N.I.S. CHY 46.1
Results and discussion
A. Calibration of 50-mL Buret
The buret that was used for the experiment was
Rotalfo, class B, and with a tolerance of ± 0. 10𝑚𝐿
𝑀𝑇 = 𝑀𝑑 + ⎡𝑀𝑑
⎣ ( 𝑃𝑎𝑖𝑟
𝑃𝐻2𝑜
−
𝑃𝑎𝑖𝑟
𝑃𝑤𝑒𝑖𝑔ℎ𝑡𝑠 )⎤⎦
• Calculation of True Volume (𝑉𝑇): Eq. 5
𝑉𝑇 =
𝑀𝑡 The mean correction factor estimated from the data
𝑃𝐻2𝑜
was 1.28 mL, which is higher than the pipette's set tolerance
• Calculation of Correction Factor (CF): Eq. 6 threshold of 0.02 ml, as shown in Table 2. Given that it
𝐶𝐹 = 𝑉𝑇 - 𝑉𝑑 failed to achieve the necessary accuracy standards for the
volumetric measurement, this demonstrates that the pipette
3 is inaccurate and inappropriate for usage. The difference
𝑃𝑎𝑖𝑟 = 1.184 kg/𝑚 or 0.001184 g/mL
between the pipette's tolerance level and correction factor
3
𝑃𝑤𝑎𝑡𝑒𝑟= 9.997.04 kg/𝑚 or 0.9970 g/mL could be caused by a variety of factors, including possible
conduct errors and procedural errors made during
𝑃𝑤𝑒𝑖𝑔ℎ𝑡𝑠= 8.4 g/mL calibration.
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Cagampang, N.I.S. CHY 46.1
Unavoidable mistakes and errors of any kind can lead
to a variety of variances in data outputs. The results of the
experiment with the calibrating buret and pipet demonstrate
a number of changes in the tolerance of the glassware itself,
as well as the cumulative correction factor of both the
calibration of the buret and pipette.
Conclusion
For precise measurements to be made in scientific
research, volumetric glassware must be calibrated. Potential
mistakes, including systematic and random errors, can be
reduced by thorough calibration, producing results that are
dependable and repeatable. For measuring liquid quantities,
volumetric glassware like burettes, pipettes, and volumetric
flasks are frequently used in laboratories. These glassware's
manufacture tolerances, however, frequently cause minor
variances in their capabilities. Consequently, calibrating
these equipment is essential to ascertain their true
capabilities.
Consequently, volumetric glassware calibration is a
necessary step. Necessary step to achieve precise and
accurate measurements in research experiments. Calibration
helps overcome inaccuracies brought on by manufacturing
tolerances for glassware and variation in operational
circumstances by addressing both systematic and random
mistakes. It is essential that labs set up a routine calibration
program to guarantee accurate and repeatable results that
increase scientific understanding.
References