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EXPERIMENT # 2
CALIBRATION OF VOLUMETRIC GLASSWARES
I. OBJECTIVES
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
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
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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
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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
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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.
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Apparent volume , mL 10 10
Correction value, mL 0 0
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Statistical Analysis
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For Table 3
( )( )
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.
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
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measurement is certain (because you are using a graduated measuring instrument). The table
showing the corrections of density and buoyancy correction is shown below.
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
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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
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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.
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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.
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
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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.
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.