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Calibration of Volumetric Glassware

The document discusses calibrating volumetric glassware like burettes, pipettes, and volumetric flasks. It describes the purpose of calibration to minimize errors and explains the procedures to calibrate different glassware. Calibration involves weighing glassware before and after adding a known volume of water to determine the actual volume. The summary is accurate.

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100% found this document useful (1 vote)
317 views7 pages

Calibration of Volumetric Glassware

The document discusses calibrating volumetric glassware like burettes, pipettes, and volumetric flasks. It describes the purpose of calibration to minimize errors and explains the procedures to calibrate different glassware. Calibration involves weighing glassware before and after adding a known volume of water to determine the actual volume. The summary is accurate.

Uploaded by

2022886536
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

ANALYTICAL CHEMISTRY

EXPERIMENT 1

CALIBRATION OF VOLUMETRIC GLASSWARE

Purpose

To learn how to do calibration of volumetric glassware in order to minimize error in


performing analysis.

Introduction

Most of the experiments in a chemistry laboratory involve careful observation and correct
laboratory techniques. It involves the use of common glassware for example burette,
pipette, volumetric flask and etc. These glassware are used to measure the volume of
solutions at certain temperature. The volume of a liquid changes with temperature, so
that to get the accuracy, the apparatus involved to measures the volume solutions have to
be calibrated before use.

Mistakes and errors can happen during an experiment. A systematic error can happen when
an apparatus which is not calibrated is used. The measurement will always be too large or
alternatively too small. A systematic error will influence the accuracy of a measurement
that is the agreement between a measured value of a quantity and its true value. Errors can
be reduced by using calibrated apparatus and being careful when doing experiment.

Volumetric flask

A volumetric flask is a glassware designed that is to prepare a standard solution at a precise


known volume of liquid at a given temperature. The actual volume of liquid in the flask can
be determined by weighing the empty flask then flask and distilled water. The difference
between both readings is equal to the mass of water. The volume of water in the flask can
be calculated from Table 1.

Pipette

Pipettes are glass vessels which are constructed and calibrated so as to quantitatively
deliver a precisely known volume of liquid at a given temperature. Two basic types of
pipettes usually found in laboratories are transfer or volumetric pipettes and measuring
or graduated pipettes. A transfer pipette is calibrated to deliver only one fixed volume,
whereas a measuring pipette is graduated so that it can deliver any volume (usually to the
nearest tenth of a milliliter) up to the maximum volume. Transfer pipettes come in many
sizes, but 5 mL, 10 mL, 20 mL and 25 mL pipettes are usually found in general chemistry
laboratories.

Step by step procedures for correct usage are:


i) Rinse the pipette with the solution to be used.
ii) Insert the pipette into the solution and suck using pipette filler (suction bulb). The
solution is about 1 to 2 cm above the etched line on the pipette.

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ANALYTICAL CHEMISTRY

iii) Drain the excess into a waste container until the bottom of the meniscus coincides with
the etched line.
iv) Allow the liquid in the pipette to drain into the flask to be used in the experiment.
Touch off the last drop. (Do not blow the remaining liquid from the pipette. The pipette
was calibrated to deliver to correct volume with this liquid remaining in it).

The actual volume of solution (pipette volume) can be measured by weighing the solution
that has been transferred using the pipette. From the density of the solution, we can
calculate the volume of solution (pipette volume).

Burette

The principal use of a burette is for the delivery of precise volume of liquid in the process
of titration. If you are using a burette for the first time, examine its marking before you fill
it. The lines that span the entire circumference occur for each milliliter, starting from zero
at the top and reaching the maximum volume at the bottom of the burette. Thus, the burette
will show the volume of a liquid that has been deliver rather than what remains. The
smaller lines each indicates tenth of a milliliter. The spacing between these lines will allow
you to estimate the volume to the nearest 0.01 ml. Thus, the typical burette readings
would be two decimal points eg. 9.34 mL or 17.60 mL. Reading such as 9.3 mL or 17.6
mL are not acceptable.

Apparatus Chemical Reagent


Analytical balance, burette, Distilled water
25 mL volumetric flask ,
20 mL or 25 mL pipette,
50 mL beaker,
Thermometer

Procedure

A. Calibration of Volumetric Flask

1. Clean and dry a 25 mL volumetric flask and weigh accurately using analytical
balance. Record the weight.
2. Fill the volumetric flask with distilled water and weigh again (use the same
balance). Record the weight.
3. Record the temperature of the distilled water.
4. From Table 1.1, determine the actual volume of the volumetric flask.

B. Calibration of Pipette

1. Clean and dry a 50 mL beaker and weigh accurately using analytical balance.
Record the weight.
2. Clean a pipette (20 mL or 25 mL) and rinse with distilled water.
3. Fill the pipette with distilled water using procedures that have been discussed in
the introduction part.
4. Drain the distilled water into the beaker and weigh again. Record the weight.
5. Repeat step 1 – 4 and record the temperature of distilled water that has been used.

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6. From Table 1, determine the actual volume of the pipette.

Table 1.1: Volume of 1 gram of Water at Various Temperatures (°C)


Temperature (°C) mL/g
24 1.0037
25 1.0039
26 1.0042
27 1.0045
28 1.0047
29 1.0050
30 1.0053
31 1.0054
32 1.0056
33 1.0058
34 1.0059
35 1.0060

Example (calculation)

Calibration of 50 mL volumetric flask:


Mass flask + water = 150.966 g
Mass empty volumetric flask = 101.385 g
Mass of water = 49.581 g

Temperature of water = 34.1 °C

From Table 1.1:


At 34 °C
If 1 g of water is equivalent to 1.0059 mL (density of water at 34°C is 1.0059 mL/g)
Therefore 49.5809 g of water is equivalent to = 49.581 g x 1.0059 mL
1g
= 49.8735 mL

The actual volume of the volumetric flask is 49.87 mL.

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ANALYTICAL CHEMISTRY

REPORT SHEET

Experiment No

Title

Name

Student ID

Course

Group

Date of Experiment

Date of Submission

Lecturer’s Name

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ANALYTICAL CHEMISTRY

EXPERIMENT 1

CALIBRATION OF VOLUMETRIC GLASSWARE

1. State the objective of the experiment.

2. Describe the procedure (in brief).

A. Calibration of Volumetric Flask

B. Calibration of Pipette

3. Results / Data

A. Calibration of Volumetric Flask

Size of volumetric flask used: …………. (mL).

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ANALYTICAL CHEMISTRY

Data table
Mass of volumetric flask
Mass of volumetric flask + water
Mass of water
Water temperature
Density of water (refer to Table 1)

Based on the data from the table above, calculate the actual volume of the
volumetric flask.

The actual volume of the volumetric flask is …………… mL

B. Calibration of Pipette

Data table
Size of pipette used: …………. (mL).

I II
Mass of beaker
Mass of beaker + water
Mass of water
Water temperature
Density of water (from Table 1)

Based on the data from the table above, calculate the actual volume of the pipette.

I II

The actual volume of the pipette


(show calculation)

Average actual volume of the pipette is ……………… mL.

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ANALYTICAL CHEMISTRY

4. Questions

a) Explain why it is necessary for a laboratory glassware such as pipette and


volumetric flask be calibrated.

b) What is the principle use of a burette? Explain how to read a burette.

c) Name the two types of pipette and explain the difference between the two.

5. Conclusion

Common questions

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The actual volume of a liquid in a volumetric flask is calculated by first weighing the empty flask and then weighing the flask filled with the liquid. The mass of the liquid is deduced by subtracting the empty flask's weight from the filled flask's weight. This mass is then converted to volume using the density of water at the recorded temperature from a reference table. For example, if the density of water is 1.0059 mL/g at 34°C, the volume of the water can be calculated by multiplying the mass by the density value .

Key procedural steps in pipette calibration include cleaning and rinsing with distilled water, ensuring freedom from contaminants, and then rinsing with the solution to be measured. The pipette's volume is calibrated by accurately weighing the transferred liquid and using the temperature-dependent density of the solution to calculate precise volume. Careful handling, such as smooth drainage and touch-off to eliminate excess, ensures the pipette delivers the intended volume, minimizing systematic errors in delivery .

Systematic errors, caused by consistent inaccuracies in equipment calibration or environmental conditions such as temperature, can result in measurements consistently deviating in one direction from the true value, affecting the accuracy. Random errors, however, are unpredictable and arise from fluctuations in experimental conditions, affecting precision rather than accuracy. In calibrating laboratory equipment, both error types can impact results. Systematic errors may be corrected through proper calibration techniques, while random errors require mitigation via repeated trials and statistical analysis to ensure reliable outcomes .

Calibration of laboratory glassware is necessary to ensure accuracy and precision in measurement. The volume of liquids changes with temperature, potentially introducing systematic errors if the apparatus are not accurately calibrated. Without calibration, measurements can consistently deviate from true values, thereby affecting analytical results. Therefore, calibration minimizes errors and enhances the reliability of experimental data .

When using a burette, it is crucial to first examine the markings that denote each milliliter and milliliter fractions, allowing precise readings to the hundredths place (e.g., 9.34 mL). Proper reading involves noting the volume delivered (rather than what remains) and estimating to the nearest 0.01 mL due to the small line spacings. Incorrect readings (such as 9.3 mL) do not yield the necessary precision for accurate titration results .

Volumetric flasks are designed to contain a precise liquid volume at a specified temperature, ensuring accurate preparation of standard solutions. Their narrow neck allows fine meniscus reading. Pipettes, particularly transfer pipettes, are calibrated to deliver an exact volume, usually with the liquid remaining, which enhances accuracy by eliminating variability in delivery volume. The design of both tools minimizes user error, offering assurance that measured solutions reflect intended volumes accurately, which is crucial for quantitative analyses in chemistry .

There are two primary types of pipettes: transfer (volumetric) pipettes and measuring (graduated) pipettes. Transfer pipettes are calibrated to deliver a single, accurate volume at a given temperature, making them ideal for tasks requiring high precision for a specific volume. In contrast, measuring pipettes are graduated, allowing the delivery of variable volumes up to their maximum capacity, typically designed for versatility rather than high precision. Each type undergoes unique calibration processes corresponding to their function .

A burette is specifically designed with markings to allow the precise delivery of a liquid through titration, enabling accurate readings to two decimal places (0.01 mL). These fine graduations ensure that small differences in volume can be precisely observed. Errors can occur if readings do not match this precision, such as improper estimation between lines or inaccurate initial zeroing. Such mistakes can lead to incorrect titrant amounts added, compromising the titration's accuracy and reliability .

Systematic errors due to incorrect calibration of volumetric glassware can consistently skew measurements either too large or too small. These errors affect the accuracy by misrepresenting the true quantity being measured. Without calibration, all subsequent measurements and analyses could be flawed, leading to misleading results and conclusions. Accurate calibration is vital to ensure that the measured values closely align with true values, minimizing this risk .

Temperature affects the density and volume of liquids; hence, a liquid's measured volume may shift with changing temperatures. During calibration, the volume of water, correlated with its mass, must be calculated based on its temperature-dependent density. Failure to account for temperature variations can lead to inaccurate calibration and significant errors in subsequent measurements. Reliable calibration requires using temperature-corrected density values to ensure accurate volume estimation .

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