Experiment 2 Calibration of Volumetric Glassware PDF

JUNE 2, 2013
CALIBRATION OF VOLUMETRIC GLASSWARE

EXPERIMENT # 2
ADORNA JR., JOEMER A.

PITAGAN, PAULA JESSIKA C.
MALAYAN COLLEGES LAGUNA
EXPERIMENT # 2
CALIBRATION OF VOLUMETRIC GLASSWARES
I. OBJECTIVES
To identify different types of volumetric glassware;

To discuss the importance of calibrating volumetric instruments;
To calibrate volumetric glassware; and
To use volumetric glassware properly.
II. LABORATORY EQUIPMENT / INSTRUMENTS / REAGENTS
Equipment/Accessories Quantity
25 mL volumetric pipet 1
10 mL volumetric pipet 1
50 mL buret 2
Aspirator 1
Analytical balance 1
Iron stand 1
50 mL beaker 2
250 mL beaker 2
125 mL Erlenmeyer flasks 2
Thermometer 1
Parafilm 1
Buret holder 1
Distilled water in wash bottle 1
III. DISCUSSION OF FUNDAMENTALS
Introduction
In the life of a simple average person, he measures everyday things with a little something
called "estimate", especially to liquids, things, and the like. But to scientists, estimation is out of the
question. Scientists, especially chemists, do not take second chances when measuring volatile
reactive liquids into their reactions. A minute addition or subtraction to it might cause explosions,
unexpected or non-visual reactions. This is very critical especially in the pharmaceutical or in the
Experiment 2: Calibration of Volumetric Glassware 1|Page

EXPERIMENT # 2
food industry. If you accidentally killed a person with a confident estimate, then chances are you are
on the verge of your pulling conscience, if you have one.
Like the first experiment, measuring volumes are as fundamental as measuring mass. But they
are a little more crucial when it comes to measuring liquid volume. Unlike solids, they more
significantly respond to changes in pressure and temperature, which is particularly dynamic, even in
a laboratory setting. In doing so, volumetric devices for measurements are used.
The type of volumetric device to be used for a particular measurement considers four factors:
general goal of the volume measurement, volume or range of volumes to be measured, degree of
reliability needed for the measurement and number of measurements to be made. Calibration of
these devices is important, as the reasons are stated above.
Theory
Volume like mass is another fundamental property of matter that is commonly determined in
analytical measurements. For solids, volume can be obtained through calculations of the objects
dimensions. For liquid materials, volume can be determined by determining the volume of the
container the liquid occupies. Most common laboratory glassware like beakers, Erlenmeyer flasks,
and test tubes serve as containers for mixing, handling, and heating solutions but are not designed
for accurate volume determinations. Volumetric devices used for analytical measurements include
volumetric flask, volumetric pipets or transfer pipet, burets, micropipets, and syringes (Hage and
Carr 2011).
Calibration of volumetric devices is very important especially when the device is recently
acquired or when the device will be used at a temperature different from the temperature it was
initially calibrated. This is because glassware will contract or expand with a change in temperature.
In addition, water expands about 0.02% per degree around 20C (Christian 2004). Therefore, the
true volume is different from the volume that is read from the container. The true volume can be
achieved by calculation considering buoyancy effects and measuring the mass of water that is
contained by the volumetric device, and then calculating the volume of water that was present
using the known density of water at that temperature (Hage and Carr 2011).
Application
Practically this experiment must be done first, among all others. This is practically because it
main application is to ensure the accuracy of the volumetric glassware, that will be frequently used

EXPERIMENT # 2
in the proceeding experiments. If this experiment gives out bad values, even though random and
systematically errors have been properly avoided and accounted for, chances are that the remaining
experiments that will follow onto this will definitely carry on this same type of error, an error that is
within the apparatus, not on the user itself.
IV. METHODOLOGY
Glasswares were cleaned with detergent

and lots of tap water. They were then
rinsed with distilled water.
200-mL distilled water was placed in a

250-mL beaker and was allowed to
equilibrate in room temperature.
Distilled water bottle was allowed to

equilibrate to room temperature. It was
used for the calibration of the burette.
Figure 2.1. Glassware and sample preparation

EXPERIMENT # 2
A clean and dry Erlenmeyer flask with a

stopper was weighed in an analytical
balance. The weight was recorded.
Actual/ true volume was taken using:
Mass of H2O with buoyancy effect = mass

of H2O * buoyancy correction (eq. 1)
Burette was filled with distilled water up
to the 0.00-mL mark. It was ensured that True volume = (corrected mass of
no leakages or bubbles were found. H2O)/(density of H2O at specified
temperature). (eq. 2)
Initial volume was read to the nearest

0.01 using a meniscus reader. Correction value for each apparent
volume was taken using:
Correction value = true volume

apparent volume (eq. 3)
About 10-mL of water was transferred
from the burette to the preweighed
Erlenmeyer flask. Delivered water =
apparent volume.
Entire procedure was repeated with 20
aliquots of water per delivery. Same was
done for 30-mL, 40-mL, and 50-mL
A stopper was put on the flask with aliquots of water.
water. Mass was recorded. Step was
repeated until water in buret was
discarded until 50-mL mark carefully.
Values were plotted: correction values on
y-axis and apparent volume on x-axis.
Differences in mass between two Figure 2.2. Calibration of 50-mL buret

consecutive mass weighings were taken
as water delivered.

EXPERIMENT # 2
For 25-mL pipet: A clean and dry 125-mL

Erlenmeyer flask with stopper was
weighed on an analytical balance.
Recorded as: initial mass. Difference in mass between each set of
two consecutive mass measurements
For 10-mL pipet: A clean, dry 50mL were obtained to determine mass of
beaker with parafilm was weighed on an
water delivered in each trial.
analytical balance. Recorded as: initial
mass.
Get true volume using eq. 1

25-mL/10-mL water was transferred from
the pipet, allowing water to run out, with
the tip of the pipet touching the side of
the beaker. It was allowed 7-10 seconds
Do entire procedure using 10-mL pipet.
to drain. The mass of the beaker and
added water was recorded. Recorded:
water delivered = apparent volume.
The following were calculated for

calibrated pipets: a. the mean volume, b.
This addition was repeated three more standard deviation, c. relative standard
times without discarding water in beaker deviation (%RSD), d. 95% confidence
or flask. Recorded for every transfer: interval, e. % relative error (theoretical
apparent volume and mass of container volume assumed was exactly 25-mL and
plus added water. 10-mL for pipets)
Figure 2.3. Calibration of 25-mL and 10-mL pipets

EXPERIMENT # 2
V. DESCRIPTION OF THE APPARATUS / SET - UP
Figure 2.4. Volumetric flask. Figure 2.5. Volumetric pipet
Figure 2.6. Burette (buret)
A volumetric flask is an instrument that is used to contain an accurate amount of liquid. A

typical volumetric flask that is used in our laboratory measures 500 mL of liquid, which has a

EXPERIMENT # 2
tolerance of 0.2 mL. This tolerance equates to a relative uncertainty of about 400 ppm (parts per
million).
A volumetric pipet is an instrument that is used to transfer accurate amounts of liquid. There
are many types of volumetric pipets, among which are used in this laboratory where the 10-mL and
the 25-mL ones. The volumetric pipet has only one graduation, and in doing so it can only deliver
one accurate measure at a time.
A burette is a laboratory apparatus that is mainly used for quantitative chemical analyses of
liquids. It consists of a long, graduated glass tube with a stopcock (in a liquid burettes case, on the
bottom) that is handled by a burette clamp, which is connected to an iron stand. The volume that
the burette dispenses is controlled by the stopcock, and is accurately measured by the graduations
of the glass tube.
VI. DATA SHEET
I. GLASSWARE AND SAMPLE PREPARATION
Table 1. Water temperature
Container Temperature (C)
250 mL beaker 24C
Distilled water bottle 24C

EXPERIMENT # 2
II. CALIBRATION OF 50 mL BURET
Table 2. Calibration of 50 mL buret
Conditions Trial 1 Trial 2
Mass of Erlenmeyer flask, g 113.79 117.52
10-mL delivery (1st)
Final volume, mL 9.9 10.0
Initial volume, mL 0.00 0.00
Volume used, mL 9.9 10.0
Mass of flask + 10 mL water, g 123.19 127.57
Mass of water, g 9.41 10.05
10-mL delivery (2nd)
10-mL delivery (3rd)

EXPERIMENT # 2
10-mL delivery (4th)
Initial volume, mL 30,0 30.0

EXPERIMENT # 2
Experiment 2: Calibration of Volumetric Glassware 10 | P a g e

EXPERIMENT # 2
Table 3. Volumes for the 50 mL Buret
Conditions Trial 1 Trial 2
Apparent volume , mL 9.9 10
Corrected mass, g 9.41 10.07
True volume, mL 9.44 10.10
Correction value, mL -0.46 0.10
Apparent volume , mL 10.1 10
True volume, mL 10,17 10.06
Correction value, mL 0.07 0.06
10-mL delivery (3rd)

EXPERIMENT # 2
Apparent volume , mL 10 10
Correction value, mL 0 0
Apparent volume , mL 10 10.1
Mass of water, g 10 10.07
Apparent volume , mL 10 9.9
Apparent volume , mL 19.9 20.0

EXPERIMENT # 2
Correction value, mL 0.03 -0.08

EXPERIMENT # 2
Correction value, mL -0.10 0.15
III. CALIBRATION OF 25 mL AND 10 mL VOLUMETRIC PIPET
Table 4. Calibration of 25 mL volumetric pipet and 10 mL measuring pipet
Conditions 25-mL pipet Conditions 10-mL pipet
Mass of Erlenmeyer 30.45

117.52 Mass of beaker, g
flask, g
25-mL delivery 10-mL delivery (1st

(1st trial) trial)
Volume delivered, mL 25.0 Volume delivered, mL 10.0
Mass of flask + 25 mL Mass of beaker + 10 40.35

142.45
water, g mL water, g
Mass of water, g 24.93 Mass of water, g 9.9
Corrected mass, g 25.02 Corrected mass, g 9.91
True volume, mL 25.04 True volume, mL 9.94
25-mL delivery 10-mL delivery (2nd

(2nd trial) trial)

EXPERIMENT # 2

167.33
25-mL delivery 10-mL delivery

(3rdtrial ) (3rdtrial)

192.21
Statistical Analysis
Average volume 25.01 Average volume 9.96
Standard deviation 0.029 Standard deviation 0.05
RSD 0.12% RSD 0.54%
95% confidence 95% confidence 9.960.049

25.010.028
interval interval
% relative error 0.04% % relative error 0.4%

EXPERIMENT # 2
VII. SAMPLE CALCULATIONS
For Table 3
( )( )
VIII. RESULTS AND DISCUSSIONS
This experiment is all about calibration of laboratory glassware. Calibration is very much
needed for the instruments, since it is one of the primary processes used in maintaining the
instruments measuring accuracy. Calibration, hence, means the process of configuring an
instrument (and accepting whatever environmental factors might be affecting it, even in a
controlled laboratory setting) to provide certain results from a sample within an acceptable range
(which is known as the tolerance). The table showing the tolerances of common Class A glassware is
shown.
Table 1. Tolerance for Class A Laboratory Glassware*

Tolerance of Class A burets Tolerance of Class A transfer pipets
Buret volume Smallest Tolerance Volume (mL) Tolerance (mL)
(mL) Graduation (mL) ((mL)
50 0.1 0.05 10 0.02
25 0.03
*Quantitative Chemical Analysis (6th ed). NY: W.H.Freeman and Company.
This is done to minimize or readily eliminate the inaccurate measurements that can be done by
the instrument, and is one of the instrumentation designs fundamental aspects. With this done, an
instrument that has assigned its proper measurement can now be called a standard. Also,
calibration is done when the environments temperature setting is not in tune with the one from
which the instrument was originally made, or formerly calibrated, since density and buoyancy
factors change the slightest of a single measurement, even though the estimated significance of the

EXPERIMENT # 2
measurement is certain (because you are using a graduated measuring instrument). The table
showing the corrections of density and buoyancy correction is shown below.
Table 2. Density of Water at Various Temperatures**
Temperature (C) Density (g/cm3) Buoyancy correction

10 0.9997026 mdisplay 1.00152
11 0.9996084 mdisplay 1.00152
12 0.9995004 mdisplay 1.00152
13 0.9993801 mdisplay 1.00152
14 0.9992744 mdisplay 1.00152
15 0.9991026 mdisplay 1.00152
16 0.9989460 mdisplay 1.00152
17 0.9987779 mdisplay 1.00153
18 0.9985986 mdisplay 1.00153
19 0.9984082 mdisplay 1.00153
20 0.9982071 mdisplay 1.00153
21 0.9979955 mdisplay 1.00153
22 0.9977735 mdisplay 1.00154
23 0.9975415 mdisplay 1.00154
24 0.9972995 mdisplay 1.00154
25 0.9970479 mdisplay 1.00155
26 0.9967867 mdisplay 1.00155
27 0.9965162 mdisplay 1.00155
28 0.9962365 mdisplay 1.00156
29 0.9959478 mdisplay 1.00156
30 0.9956502 mdisplay 1.00156
** All of the densities shown for pure air-free water at a pressure of 101.325 kPa (1 atm). The
buoyancy corrections assume that the air density is 1.20 x 10-3 g/cm3 and the density of the reference
weight is 8.00 g/cm3.
** Analytical Chemistry and Quantitative Analysis. New Jersey: Pearson Prentice Hall.
We started the experiment off by thoroughly cleaning the glassware. They are clean as it
seems, but maybe the students that used it before us didnt thoroughly clean it through, so we have
to do it again for assurance that the calibration will be very much accurate. The final rinsing will be

EXPERIMENT # 2
the distilled water, which is free of most ions present in tap water, and in effect the water will not
be attracted to the sides of the glassware, creating a free flowing liquid inside. Since the distilled
water that we used in the wash bottle already equilibrated to room temperature, we just read this
temperature which will be used for computations later on.
We started calibrating the 50-mL buret by filling the buret with distilled water. Then, by getting
the mass of the Erlenmeyer flask (which will be used throughout this whole procedure) we now
transfer an appropriate amount (10-ml aliquots, adding 10 to the preceding one until we have 50-
mL aliquots, for two trials) to the flask and weigh the flask. The difference between the last reading
and the initial will be the mass of the water. After all trials and different aliquots have been done,
we go to the computation step. By having the apparent mass of the water, we now compute for the
corrected mass of water by the equation:
( )( ). (Eq 1)
By getting the mass, we can get the corrected/true volume by the equation:
. (Eq 2)
By having the true volume, we compute for the correction value as follows:
. (Eq 3)
After this, we will graph the correction values vs. apparent volume. By inspection, you can see
that there are negative and positive values for the correction value. This is mainly because of the
difference in the mass weighed to the volume that you have estimated to the burettes significant
figures (even with the help of the meniscus reader). The slope of the line will serve as the relative
error of the calibration process, and if it goes by the specific tolerance, then the glassware has been
properly calibrated.
For the calibration of the 10-mL and 25-mL pipet, a proper container for delivery is allocated
for the different measuring instruments. A 125-mL E. flask is used for the 25-mL pipet and a 50-mL
beaker with parafilm for the 10-mL pipet. By getting the respective weights of the containers, for
three trials we transferred distilled water to its appropriate container, and weighing it to get the
difference, which will serve as the apparent mass of water. After all trials have been made, the
computation process will be the same as the 50-mL buret computations, i.e. getting the correction

EXPERIMENT # 2
value. After this has been made, the data that we have computed and determined will be compared
using statistical analysis. By getting the means of the true volumes of the different pipets, we
computed for the standard deviation by the equation:
( )
. (Eq 4)
After that, we computed for the coefficient of variation (%relative standard deviation) to see
how precise our measurements are. We got a low value; therefore our precision is very high. Also,
the %RSD can be used as comparison for the tolerances that is in Table 1. From what we got, we are
inside the bounds of the tolerance values, therefore the values are within range. By getting the
confidence interval, we computed for its actual tolerances, assuming that this is the working
temperature for this glassware throughout the whole term. Lastly, we determined the %relative
error, using 25-mL and 10-mL measurements as the theoretical volume. This can be compared to
the tolerances, and from what we got, we are within range.
10-mL aliquots (Correction values vs. Apparent

volume)
0.12
y = 2x - 19.92
0.1 0.1
0.08
Correction values
0.06 0.06
0.04 Linear (Correction
values)
0.02
0 0
9.94 9.96 9.98 10 10.02
-0.02

EXPERIMENT # 2
20-mL aliquots (Correction values vs. Apparent

volume)
0.1
0.09
0.08 y = 0.3x - 5.97
0.06
Correction values
0.04
0.03
0.02 Linear (Correction
values)
0
19.85 19.9 19.95 20 20.05 20.1 20.15
-0.02
-0.03
-0.04
By cleaning up everything and putting everything to what it was back before, we conclude the
experiment to a finish.
IX. SUMMARY AND CONCLUSIONS
This experiment verified the concept involving the how tos of calibrating glassware, such as
burettes and volumetric flasks. The glasswares were already previously calibrated during
manufacture by the Quality Control (QC) department, but calibrating the instruments would be
needed to ensure that no errors have been made by the QC, if ever. Even in a controlled laboratory
setting, a random error can always happen.
Certain factors that can affect the precision and accuracy of measurements of these glasswares
are quite a few. Linear expansion would b a thing, but since the difference in the temperature in the
laboratory would be very low, this can be way much disregarded. A difference in temperature, from
what is said earlier, however, can affect the density of the liquid being contained or transferred.
Density is the mass to volume ratio of a substance i.e. liquid, which is significant since for every
degree of change, there would be a notable difference in the density. This is because the mass of

EXPERIMENT # 2
the water is affected by buoyancy. With this changes, plus environmental factors, will cause a
significant change between the volume obtained, and the true volume.
Overall, by getting the relative difference through statistical methods and comparing it to the
standard values (with the tolerance values as a guide for maximum allowable error), if it is within
the bounds, then we can conclude that the glassware are calibrated to accuracy, and can be used for
future purposes.
X. POST LAB QUESTIONS
1. What is the maximum allowable error for the respective volumetric glassware that you
calibrated?
Based on our data, the maximum allowable error is about 0.41%, since the average tells this
much difference, as to the computation o the relative error.
2. Are your errors within the tolerance volumes for the Class A glassware? What are the
systematic or random errors that have occurred?
Yes. If there are errors, what have possibly occurred would be: the reading of the lower
meniscus, which always results to estimation; and possibly the water drops left inside the
glassware due to the surface tension inside.
XI. REFERENCES
Christian, Gary D. 2004. Analytical chemistry (6th ed.). John Wiley and Sons Inc.
Hage, David S. and James D. Carr. 2011. Analytical chemistry and quantitative analysis. New
Jersey: Pearson Prentice Hall.
Skoog, Douglas et. al. 2004. Fundamentals of Analytical Chemistry (8th ed.). Singapore:
Thomson Learning.

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JUNE 2, 2013

CALIBRATION OF VOLUMETRIC GLASSWARE

ADORNA JR., JOEMER A.

To identify different types of volumetric glassware;

II. LABORATORY EQUIPMENT / INSTRUMENTS / REAGENTS

III. DISCUSSION OF FUNDAMENTALS

Experiment 2: Calibration of Volumetric Glassware 1|Page

Experiment 2: Calibration of Volumetric Glassware 2|Page

Glasswares were cleaned with detergent

200-mL distilled water was placed in a

Distilled water bottle was allowed to

Experiment 2: Calibration of Volumetric Glassware 3|Page

A clean and dry Erlenmeyer flask with a

Mass of H2O with buoyancy effect = mass

Initial volume was read to the nearest

Correction value = true volume

Differences in mass between two Figure 2.2. Calibration of 50-mL buret

Experiment 2: Calibration of Volumetric Glassware 4|Page

For 25-mL pipet: A clean and dry 125-mL

Get true volume using eq. 1

The following were calculated for

Figure 2.3. Calibration of 25-mL and 10-mL pipets

Experiment 2: Calibration of Volumetric Glassware 5|Page

V. DESCRIPTION OF THE APPARATUS / SET - UP

Figure 2.4. Volumetric flask. Figure 2.5. Volumetric pipet

Figure 2.6. Burette (buret)

A volumetric flask is an instrument that is used to contain an accurate amount of liquid. A

Experiment 2: Calibration of Volumetric Glassware 6|Page

VI. DATA SHEET

I. GLASSWARE AND SAMPLE PREPARATION

Table 1. Water temperature

Container Temperature (C)

250 mL beaker 24C

Distilled water bottle 24C

Experiment 2: Calibration of Volumetric Glassware 7|Page

II. CALIBRATION OF 50 mL BURET

Table 2. Calibration of 50 mL buret

Conditions Trial 1 Trial 2

Mass of Erlenmeyer flask, g 113.79 117.52

10-mL delivery (1st)

Final volume, mL 9.9 10.0

Initial volume, mL 0.00 0.00

Volume used, mL 9.9 10.0

Mass of flask + 10 mL water, g 123.19 127.57

Mass of water, g 9.41 10.05

10-mL delivery (2nd)

Final volume, mL 20.0 20.0

Initial volume, mL 9.9 10.0

Volume used, mL 10.1 10.0

Mass of flask + 10 mL water, g 133.2 137.59

Mass of water, g 10.05 10.02

10-mL delivery (3rd)

Final volume, mL 30.0 30.0

Initial volume, mL 20.0 20.0

Volume used, mL 10.0 10.0

Mass of flask + 10 mL water, g 143.28 147.54

Experiment 2: Calibration of Volumetric Glassware 8|Page

Mass of water, g 9.96 9.95

10-mL delivery (4th)

Final volume, mL 40.0 40.1

Initial volume, mL 30,0 30.0

Volume used, mL 10.0 10.1

Mass of flask + 10 mL water, g 153.28 157.61