Experiment 1- Glassware and Uncertainty

Experiment 1: The Use of Volumetric Glassware

and it’s Uncertainty
Objectives
• To gain familiarity with the various instruments used for making physical measurements in the
laboratory, which are essential to the study of experimental chemistry. In this experiment, you
will investigate the uses and limits of the various types of volumetric glassware commonly
encountered in a chemistry lab.

Introduction

Most of the glassware in the laboratory has been marked by the manufacturer to indicate the
volume contained by the glassware when filled to a certain level. The markings, or what are
referred to as “graduations” are etched or painted onto the glassware by the manufacturer.
These graduations differ greatly in the precision they indicate depending on the type of
glassware and its intended use. For example, beakers and Erlenmeyer flasks are marked with
very approximate volumes, which serve merely as a rough guide to the volume of liquid in the
container. Other pieces of glassware, notably burets, pipets, and graduated cylinders, are
marked much more precisely by the manufacturer and are used to measure more precise
volumes. It is important to distinguish when a precise volume determination is necessary and
appropriate for an experiment and when only a rough determination of volume is needed. It is
also important to understand how to read each piece of glassware and to determine and
understand the uncertainty associated with each type of glassware.

A. Graduated Cylinders
The most common apparatus for routine determination of liquid volumes is the graduated
cylinder. Although a graduated cylinder does not permit as precise a determination of volume
as do other volumetric devices, for many applications the precision of the graduated cylinder is
sufficient.

Figures 2-1 and 2-2 show typical graduated cylinders. In Figure 2-1, notice the plastic safety
ring, which helps to keep the graduated
cylinder from breaking if it is tipped over.
In Figure 2-2, compare the difference in
graduations shown for the 10-mL and 100-
mL cylinders. Examine the graduated
cylinders in the lab and determine the
smallest graduation of volume that can
determine with each cylinder.

1
Experiment 1- Glassware and Uncertainty

When water (or an aqueous solution) is contained in a narrow glass container such as a
graduated cylinder, the liquid surface is not flat, as might be expected. Rather, the liquid
surface is curved downward (see Figure 2-3). This curved surface is called a meniscus and is
caused by an interaction between the water molecules and the molecules of the glass container
wall. When reading the volume of a liquid that makes a meniscus, hold the gradated cylinder so
that the meniscus is at eye level, and read the liquid level at the bottom of the curved surface
(that is, tangent to the curved surface).

B. Pipets

When a more precise determination of liquid volume is needed than can be provided by a
graduated cylinder, a transfer pipet may be used. Pipets are especially useful if several
measurements of the same volume are needed (such as in preparing similar-sized samples of a
liquid substance). Two types of pipets are commonly available, as indicated in

Figure 2-4. The Mohr pipet is calibrated, at least, at each milliliter and can be used to deliver
any size sample (up to the capacity of the pipet). The volumetric transfer pipet can deliver only
one size sample (as stamped on the barrel of the pipet and indicated by the line towards the
top of the pipet), but generally it is easier to use and the results are more reproducible.

Pipets are filled using a rubber safety bulb to supply the suction needed to draw liquid into the
pipet. It is absolutely forbidden to pipet by mouth in the chemistry laboratory. Two common
types of rubber safety bulbs are shown in Figure 2-5.

2
Experiment 1- Glassware and Uncertainty

The simple bulb should not actually be placed onto the barrel of the pipet. This would be likely
to cause the liquid being measured to be sucked into the bulb itself. Rather, squeeze the bulb,
and just gently press the opening of the bulb against the opening in the barrel of the pipet to
apply the suction force, keeping the tip of the pipet under the surface of the liquid being
sampled. Do not force the pipet into the plastic tip of the safety bulb, or the pipet may break.
Allow the suction to draw liquid into the pipet until the liquid level is 1 or 2 inches above the
calibration mark on the barrel of the pipet. At this point, quickly place your index finger or
thumb over the opening at the top of the pipet to prevent the liquid level from falling. By
gently releasing the pressure of your finger, you can allow the liquid level to fall until it reaches
the calibration mark of the pipet. The tip of the pipet may then be inserted into the container
that is to receive the sample and the pressure of the finger removed to allow the liquid to flow
from the barrel of the pipet. (See Figure 2-6.)

3
Experiment 1- Glassware and Uncertainty

Finally, glassware is intended to contain or to deliver specific volumes and is generally marked
on the glassware with the markings “TC” (to contain) and “TD” (to deliver). They may sound the
same, but please keep in mind there is a slight difference. A flask or beaker would be marked as
TC, implying that it contains a specific amount of liquid. A pipet on the other hand is designed
to deliver a very accurate and precise amount, so a pipet marked “TD 10 mL” will deliver 10.00
mL of liquid. The remaining liquid in the tip is there by design; 10.00 mL has been delivered to
the container and any remaining liquid in the tip is not needed. So, when using a pipet, it’s very
important to recognize the last remaining liquid is supposed to remain there, don’t force it out.

When using either type of pipet, observe the following rules:

1. The pipet must be scrupulously clean before use: wash with water, rinse with tap water,
and then rinse with distilled water. If the pipet is clean enough for use, the water will not
bead up anywhere on the inside of the barrel.
2. To remove rinse water from the pipet (to prevent dilution of the solution to be measured),
Do not to be measured, discarding the rinses in a waste beaker for disposal. It is not
necessary to fill the pipet completely with the solution for rinsing.
3. The tip of the pipet must be kept under the surface of the liquid being measured out
during the entire time suction is being applied, or air will be sucked into the pipet.
4. Allow the pipet to drain for at least a minute when emptying to make certain the full
capacity of the pipet has been delivered. Remove any drops of liquid adhering to the tip of
the pipet by touching the tip of the pipet to the side of the vessel that is receiving the
sample. Do not force any remaining liquid out of the pipet tip (this is allowed for in the
calibration of the pipet).
5. If you are using the same pipet to measure out several different liquids, you should rinse
the pipet with distilled water between liquids and follow with a rinse of several small
portions of the next liquid to be measured.

C. Burets

When samples of various sizes must be dispensed or measured precisely, a buret may be used.
The buret consists of tall, narrow calibrated glass tube, fitted at the bottom with a valve for
controlling the flow of the liquid. The valve is more commonly called a stopcock (See Figure 2-7.)

Like a pipet, a buret must be scrupulously clean before use. The precision permitted in reading
a buret is 0.02 mL, but if the buret is not completely clean, this level of precision is not
attainable. Rinse the buret with tap water, followed by several rinsing with distilled water.
Before use, the buret should be rinsed with several small portions of the solution to be used in
the buret. The buret should be tilted and rotated during the rinsing, to make sure that all rinse
water is washed from it. Discard the rinsing. After use, the buret should again be rinsed with
distilled water. Many of the reagent solutions used in burets may attack the glass of the buret if
they are not removed, which would destroy the calibration. Make sure when filling the buret a
funnel is used and the top of the buret is brought down to eye level (typically by carefully
allowing the tip to hang off the bench top) so you are not pouring liquids over your head.

4
Experiment 1- Glassware and Uncertainty

A common mistake made by beginning students is to fill the buret with the reagent solution to
be dispensed to exactly the 0.00 mL mark. This is not necessary or desirable in most
experiments, and it wastes time. The buret should be filled to a level that is comfortable for
you to read (based on your height). A precise initial liquid-level reading of the buret should be
taken before the solution is dispensed and again after the liquid is dispensed. The readings
should be made to the nearest 0.01 mL. The volume of liquid dispensed is then obtained by
simple subtraction of the two volume readings. Always use a funnel when filling a buret, and
always have the buret top below the eye level when you are adding liquid.

Data Analysis

Density calculations:
In several places in the experiment, you will be asked to use the Water Density Table which
lists the density of water at various temperatures, so you can compare the volume as delivered
by the particular type of glassware (this is what you observed during the experiment, quick, but
not as accurate), with the volume calculated from the mass of the water transferred (calculation
offers much better precision, but requires more time in the lab). Since the determination of
mass is typically more precise than the determination of volume, this serves as a check on the
calibration marks on the glassware, and also on your skill in using them.

Volume delivered vs Volume calculated:

From the glassware using the formula & density of water
𝑚𝑚
𝑑𝑑 =
.
𝑉𝑉
Suppose we measure the mass of a “5 mL” sample of water at 22°C and find it weighs 5.015 g.
Using the density of water at 22°C from the Water Density Table (0.99780 g/mL), the calculated
volume of the sample would be: Volume = mass/density = (5.015g)/(0.99780g/mL) = 5.026 mL

5
Experiment 1- Glassware and Uncertainty

Percentage Error
Percentage error is a way to check your experimental technique as well as the equipment used,
against what is accepted by the scientific community. The percent error is based on the
experimentally determined values obtained by a student in the lab, against the literature values
accepted by science. If percent error is high, that is an indication that there is an experimental
issue: human error as a result of poor technique or flawed equipment providing inaccurate
measurements; most often it’s a combination of the two.

|𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣 − 𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣|

% 𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒 = 𝑥𝑥100
𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙𝑙 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣

For this lab, the experimental value is equivalent to the observed value in the data table. The
literature value is equivalent to the calculated value in the data table, which was found by using
the literature value of density and calculating the volume. See equation below for clarity:

|𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜𝑜 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣 − 𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣|

% 𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒 = 𝑥𝑥100
𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐𝑐 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣

6
Experiment 1- Glassware and Uncertainty

Procedure

Record all data and observations in the space provided below, please write legibly.

Materials/Reagents Required
• 25 mL graduated cylinder • distilled water squeeze bottles
• 10 mL volumetric pipet and safety bulb • thermometer
• buret with clamp & stand • 125 mL Erlenmeyer flask
• funnel (for filling buret)
• 50 mL and 150 mL beakers

A. The Graduated Cylinder

Part I: In the lab, there will be a display of several graduated cylinders filled with different
amount of colored water. Several sizes of cylinders are available (10-mL, 25-mL, 50-mL, and
100-mL).

1. Examine each cylinder, paying particular attention to the marked scale divisions on the
cylinder.
2. Read and record the volume of liquid contained in each graduated cylinder. Make the
volume readings to the level of precision permitted by each of the cylinders (e.g. add
one uncertain digit). Record your readings in the table labeled “Graduated Cylinder” in
the data section.

Check your readings of the liquid levels with the instructor before proceeding. Ask for
assistance if your readings differ from those provided by the instructor.

Part II: Fill the 150 mL Beaker about half way with distilled water, place a thermometer in it
and set it on the lab bench top.

1. Clean and wipe dry a 25-mL graduated cylinder and a 50-mL beaker (a rolled-up paper
towel will enable you to dry the interior of the graduate). Weigh the empty beaker and
record the mass to three decimal places. Record this value as “Mass of Beaker (empty)”
in the data section.

2. Fill the 25-mL graduated cylinder with 10 mL distilled water, from the 150 mL beaker,
so that the meniscus of the water level lines up right around the 10-mL calibration mark
of the cylinder. Read and record the volume in the graduated cylinder to the correct
number of significant digits. Record this value as “Volume of Water (observed)” in the
data section.

7
Experiment 1- Glassware and Uncertainty

3. Pour the distilled water from the graduated cylinder into the 50-mL beaker. (DO NOT
add water while it’s on the balance).

4. Weigh the 50-mL beaker, with the water, and record the mass to three decimal places.
Record this value as “Mass of Beaker + Water” in the data section.

5. Calculate the mass of the water delivered (by subtracting the mass of the empty beaker
from the mass of the beak + water) and record this value as “Mass of Water” in the data
section.

6. Look up the density of water at the temperature your thermometer is reading. This can
be done using the Density of Water table from the CRC Handbook (located on the backs
of the pillars in the lab and below in this handout).

7. Next, calculate the volume of water present in the graduated cylinder and beaker from
the exact mass of water present in each. Record this value as “Volume of Water
(calculated)” in the data section. You will need to record the water temperature to
correctly use the CRC Handbook.

8. Compare the calculated volume of water (based on the mass of water) to the observed
volumes of water determined from the calibration marks on the cylinder and beaker.
Calculate the percentage difference (% error) between the calculated volume and the
observed volume from the calibration marks.

B. The Pipet

Obtain a 10-mL volumetric pipet and rubber safety bulb. Clean the pipet with tap water
followed by distilled water. Using the water from the 150 mL beaker, practice filling and
dispensing distilled water from the pipet until you feel comfortable with the technique. Ask
your instructor for assistance if you have any difficulties in the manipulation.

1. Wipe dry the 50-mL beaker. Weigh the beaker and record the mass to three decimal
places. Record this value as “Mass of Beaker (empty)” in the data section.

2. Pipet 10.00 mL of the distilled water, from the 150 mL beaker, into the clean beaker
you have weighed. Record this value as “Volume of Water (observed)” in the data
section.

3. Weigh the 50-mL beaker, with the water, and record the mass to three decimal places.
Record this value as “Mass of Beaker + Water” in the data section.

4. Calculate the mass of the water delivered and record this value as “Mass of Water” in
the data section.

8
Experiment 1- Glassware and Uncertainty

5. Using the Density of Water table in the CRC Handbook, calculate the volume of water
present in the graduated cylinder and beaker from the exact mass of water present in
each. Record this value as “Volume of Water (calculated)” in the data section. You will
need to record the water temperature to correctly use the CRC Handbook.

6. Compare the calculated volume of water (based on the mass of water) to the observed
volumes of water determined from the calibration marks on the cylinder and beaker.
Calculate the percentage difference (% error) between the calculated volume and the
observed volume from the calibration marks.

Compare this calculated volume to the volume of the pipet as specified by the manufacturer.
Any significant difference between these two volumes is an indication that you need additional
practice in pipeting. Consult with your instructor for help.

C. The Buret

Obtain a buret and place it in a clamp on the lab bench. Be sure it is perfectly perpendicular to
the benchtop. Fill the buret with tap water and check to make sure that there are no leaks from
the stopcock before proceeding. If the stopcock leaks, have the instructor examine the stopcock
to make sure that all the appropriate washers are present. If the stopcock cannot be made leak
proof, replace the buret. Drain the tap water.

Fill the buret to above the zero mark with distilled water, after washing as discussed earlier.
Open the stopcock of the buret and allow the distilled water to run from the buret into a
beaker or flask. Examine the buret while the water is running from it. If the buret is clean
enough for use, water will flow in sheets down the inside surface of the buret without beading
up anywhere. If the buret is not clean, rewash it.

1. Refill the buret with distilled water to a point somewhat below the zero mark.
Determine the precise liquid level in the buret to the correct number of significant
figures (nearest 0.01 mL). Record this value as “Volume of Water (initial)” in the data
section.

2. Clean and wipe dry a 50-mL beaker. Weigh the beaker and record the mass to three
decimal places. Record this value as “Mass of Beaker (empty)” in the data section.

3. Place the weighted beaker beneath the stopcock of the buret. Open the stopcock of the
buret and run water into the beaker until approximately 10.00 mL of distilled water has
been dispensed. Determine the precise liquid level in the buret to the nearest 0.01 mL.
Record this value as “Volume of Water (final)” in the data section

4. Calculate the volume of water that has been dispensed from the buret by subtraction of
(final volume – initial volume) = total volume delivered. Record this value as “Volume
of Water (observed)” in the data section.

9
Experiment 1- Glassware and Uncertainty

5. Weigh the 50-mL beaker, with the water, and record the mass to three decimal places.
Record this value as “Mass of Beaker + Water” in the data section.

6. Calculate the mass of the water delivered and record this value as “Mass of Water” in
the data section.

7. Using the CRC Handbook, calculate the volume of water present in the graduated
cylinder and beaker from the exact mass of water present in each. Record this value as
“Volume of Water (calculated)” in the data section. You will need to record the water
temperature to correctly use the CRC Handbook.

8. Compare the calculated volume of water (based on the mass of water) to the observed
volumes of water determined from the calibration marks on the cylinder and beaker.
Calculate the percentage difference (% error) between the calculated volume and the
observed volume from the calibration marks.

Compare the volume of water transferred (as determined by reading the buret) with the
calculated volume of water (from the mass determinations). If there is any significant
difference between the two volumes, you probably need additional practice in the operation
and reading of the buret.

10
Experiment 1- Glassware and Uncertainty

Name: __________________________________ Date: __________________ Section: _______

Pre-Laboratory Assignment: Glassware and Uncertainty

1. Purpose/Objective:

2. What is a meniscus? How do we typically read the liquid level when dealing with a liquid
that forms a meniscus?

3. It is important to make certain that there is no air bubble in the tip of the buret below the
stopcock before the initial reading of the liquid level in the buret is taken. If a 0.5-mL air
bubble is present in the tip of a buret, calculate what percent error in a 40-mL sample will
result if the air bubble is dislodged during the dispensing of the sample?

11
Experiment 1- Glassware and Uncertainty

Name: _______________________________ Partner: _______________________________

Date: _________________ Section: _________

Data Sheets: Glassware and Uncertainty (Watch significant figures!)

A. The Graduated Cylinder

Part I:

Liquid Color Volume (mL) Uncertainty

Check your readings of the liquid levels with the instructor before proceeding

Part II:
Trial 1 Trial 2 Trial 3

Mass of Beaker + Water (g): __________ __________ __________

Mass of Beaker (empty) (g): __________ __________ __________

Mass of Water (g): __________ __________ __________

Volume of Water (observed) (mL): __________ __________ __________

Water Temperature (°C) __________ __________ __________

B. The Pipet
Trial 1 Trial 2 Trial 3

Mass of Beaker + Water (g): __________ __________ __________

Mass of Beaker (empty) (g): __________ __________ __________

Mass of Water (g): __________ __________ __________

Volume of Water (observed) (mL): __________ __________ __________

Water Temperature (°C) __________ __________ __________

12
Experiment 1- Glassware and Uncertainty

C. The Buret
Trial 1 Trial 2 Trial 3
Volume of Water (final) (mL): __________ __________ __________
Volume of Water (initial) (mL): __________ __________ __________
Volume of Water (observed) (mL): __________ __________ __________
Mass of Beaker + Water (g): __________ __________ __________
Mass of Beaker (empty) (g): __________ __________ __________
Mass of Water (g): __________ __________ __________
Water Temperature (°C) __________ __________ __________

Instructor Signature:

13
 Experiment 1- Glassware and Uncertainty

Name: _______________________________ Partner: _______________________________

Date: _________________ Section: _________

Post-Laboratory Assignment: Glassware and Uncertainty

I. Calculations: Use the data collected to show the work in detail (proper setup and units)
for all the questions below. Report the answers using proper significant digits and units.

A. The Graduated Cylinder-Part II

a) Look up the true density of water at the temperature recorded (from CRC Handbook):

b) Calculate the volume of water using the mass of water obtained in the lab (data collected)
and the true value of density of water (from question a above). Show the calculation for the
first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

c) Calculate the average volume of water using the values from part b above.

d) For each trial: Use the observed value of the volume of water (from the data table) and the
calculated value (part c above) to calculate the percent error in volume of water.

|observed value − calculated value|

% error = x100
calculated value

14
Experiment 1- Glassware and Uncertainty

Show the calculation for the first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

e) Calculate the average % Error

B. The Pipet

a) Look up the true density of water at the temperature recorded (from CRC Handbook):

b) Calculate the volume of water using the mass of water obtained in the lab (data collected)
and the true value of density of water (from question a above). Show the calculation for the
first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

c) Calculate the average volume of water using the values from part b above.

15
Experiment 1- Glassware and Uncertainty

d) For each trial: Use the observed value of the volume of water (from the data table) and the
calculated value (part c above) to calculate the percent error in volume of water.

|observed value − calculated value|

% error = x100
calculated value

Show the calculation for the first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

e) Calculate the average % Error

C. The Buret

a) Look up the true density of water at the temperature recorded (from CRC Handbook):

b) Calculate the volume of water using the mass of water obtained in the lab (data collected)
and the true value of density of water (from question a above). Show the calculation for the
first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

16
 Experiment 1- Glassware and Uncertainty

c) Calculate the average volume of water using the values from part b above.

d) For each trial: Use the observed value of the volume of water (from the data table) and the
calculated value (part c above) to calculate the percent error in volume of water.

|observed value − calculated value|

% error = x100
calculated value

Show the calculation for the first trial and write the answers for the remaining trials.

Trial 1:

Trial 2:

Trial 3:

e) Calculate the average % Error

II. Results (summarize findings in the table below)

A. Graduated A. Graduated B. Pipet C. Buret

Cylinder Cylinder
(Part 1) (Part 2)
1. Observed volume Average volume of Average volume of Average volume of
water calculated water calculated water calculated
_______________

Uncertainty ______________ ______________ ______________

_________

2. Observed volume

_______________ Average % error Average % error Average % error

_____________ _____________ _____________

Uncertainty
_________

17
 Experiment 1- Glassware and Uncertainty

III. Discussion:
Use the calculated values of your results in this experiment, briefly discuss the relative precision
permitted by a graduated cylinder, a pipet, and a buret. Explain the errors and how they could be
improved.

IV. Conclusion: Give your conclusion(s) of the overall experiment.

18
 Experiment 1- Glassware and Uncertainty

V. Post-lab Questions:

1. Define the following:

a. Precision –

b. Accuracy –

c. % error –

2. Suppose a 1.0 mL air bubble is trapped in the tip of your buret and you don’t notice it before
measuring out liquid samples with the buret. What percentage error would be introduced in a 35.0
mL sample of liquid if the air bubble comes out of the tip of the buret while the liquid sample is
being transferred? (Show work)

19