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INTRODUCTION TO ANALYTICAL CHEMISTRY – LAB

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EXPERIMENT 1

INTRODUCTION TO THE ANALYTICAL LABORATORY –


DETERMINATION OF MASS AND VOLUME

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MEASUREMENT OF MASS USING THE ANALYTICAL BALANCE

INTRODUCTION

The purpose of this experiment is, first and foremost, to familiarize you with the operation of the
analytical balance. Because all analytical determinations are (directly or indirectly) based on the
measurement of mass, learning the correct balance technique is vital to the success of your
experiments. Additionally, you will use the balance to demonstrate the need to dry samples and
standards prior to analysis.

THE ANALYTICAL BALANCE

General rules for use of the analytical balances

1. Keep the balance clean. Remove dust, etc. from the pans with a camel-hair brush.
2. Learn the capacity of your balance, and never exceed this capacity.
3. Objects to be weighed should be at room temperature.
4. Strategies must be developed to ensure that moisture is not transferred to the object being
weighed during handling.
5. Do not rub or polish objects before weighing.
6. Chemicals are never placed directly on the balance pan. Use a weighing bottle, beaker,
watchglass, etc.
7. After you have completed weighing, check the following:
a) You have recorded your results correctly.
b) The balance pan is clean.
c) There are no objects left on the pan.
8. Corrosive liquids and solids are always placed in a vapor tight, pre-weighed container
before weighing on an analytical balance.
9. Report and record anything unusual.

The Sartorius Balance

An analytical balance is one which weighs to ± 0.1mg and has a maximum capacity of ~200g. A
number of companies produce reliable, rugged and reproductible analytical balances. The
balances in the laboratory are Sartorius Balances (produced by the Sartorius Company). They
are accurate to ± 0.1mg and have a maximum capacity of 210g.
PART I: PROCEDURE FOR OBTAINING THE MASS OF AN OBJECT

Using analytical instrumentation correctly requires practice. This exercise will give you the
opportunity to develop confidence in your weighing skills.

1. Check the zero load before and after each weighing.


2. Determine the weight of a clean, dry, weighing bottle (without lid) to within +0.1 mg.
Caution: Do not handle the glassware with your fingers (or thumbs or toes) unless otherwise
instructed.
3. Determine the weight of the weighing bottle lid to within +0.1 mg.
4. Determine the total weight of the weighing bottle plus lid to within +0.1 mg.
5. Repeat steps 2-4 at least two more times to demonstrate the reproducibility of these
measurements.
6. Make sure you have recorded all your data in your laboratory notebook.

Compare the sum of the weights of the weighing bottle and lid determined separately with
the weight of the lid and bottle determined together. Explain any discrepancies between the
weights that you find. Suggest using your data a value that is most likely to be closest to the
“real true weight” for this series of experiments.

PART II: DETERMINING THE EFFECT OF ENVIRONMENTAL CONDITIONS ON


THE MEASUREMENT OF MASS

Measuring the mass of objects that are either significantly hotter or colder than ambient
temperature will produce errors similar to those you would observe if you forgot to close the
doors on the balance. The cause is similar, air currents exerting an upward or downward
force on the balance pan, making the object appear to weigh less (or more) than its true
value, depending on the direction of the force. Additionally, unintended moisture can alter
the apparent mass of an object as well.

1. Heat a weighing bottle in the microwave oven at medium power for 2 minutes. Quickly
weigh the hot weighing bottle and record your initial weight. (NOTE: The reading on the
balance may be unstable while you take the measurement.)
2. Remove the hot weighing bottle from the balance and place it in your desiccator to cool for
approximately ten minutes. After the weighing bottle has cooled, again determine its weight
to within ± 0.1 mg.
3. Remove the weighing bottle from the balance and roll it in your hands. Leave it to stand on
the laboratory bench for five minutes and weigh.
4. Hold the weighing bottle near your mouth and breathe onto it several times. Reweigh the
weighing bottle.
Suggest using your data a value that is most likely to be closest to the “real true weight” for
this series of experiments. Compare the weights of the weighing bottle determined under
differing conditions with the value you think is closest to the "real true weight" and explain
the possible sources and reasons for any observed discrepancies. Compare the “real true
weights” from parts I and II and again explain any discrepancies. You will find it helpful to
record your data in table form. A spreadsheet, such as EXCEL, is particularly useful, as it
facilitates calculations directly from the data.
PRECISION AND ACCURACY OF COMMON ANALYTICAL GLASSWARE - PIPETS
AND VOLUMETRIC FLASKS

INTRODUCTION

Pipets and volumetric flasks are basic laboratory equipment designed to accurately deliver (the
pipet) or contain (the volumetric flask) a desired volume of pure liquid or liquid solution. For
this reason, knowledge of the precision (measured as reproducibility) and the error (measured in
terms of accuracy or tolerance) associated with specific pipets and volumetric flasks is important.
Remember, each measurement and measuring device contributes to the total uncertainty of the
final result of an analytical determination.

Accuracy is defined as a measure of how close a measured value is to the “real true” value.
Accuracy is often described in terms of its absence, error. Tolerance is the manufacturers stated
uncertainty in the accuracy of a measuring device. Precision is a measure of the reproducibility
of a measurement. It is very important to remember that the skill of the operator, as well as the
quality of the measuring device, determine the quality of the final result.

Both precision and accuracy of a pipet or volumetric flask is determined through a mass
measurement. For the pipet successive aliquots of deionized water are weighed and converted to
a volume using the density of water at the temperature of the water. The precision and accuracy
associated with the individual pipet is then determined. A similar technique is used for the
volumetric flask where the difference in weight between an empty and full flask is determined
and converted to a volume using the density of the water at the temperature of the water. Again,
from these results the precision and accuracy associated with an individual volumetric flask are
calculated. Performing a number of replicate determinations allows the estimation of the central
tendency and confidence limits associated with the measurement.

Your objective in this experiment is to become proficient in the use of these measuring devices.
You should perform a sufficient number of replicate determinations to ensure that you are both
competent and confident in your ability to use these devices to their full potential.

PROCEDURE

You are responsible for determining the precision and accuracy of three pieces of volumetric
ware: a 5-mL volumetric pipet, a 5-mL Eppendorf pipet, and a 50-mL volumetric flask.

The 5-mL Volumetric Pipet

1. Before starting the experiment ensure that your pipet is clean (no beading of water is
observed when water is delivered from the pipet). Clean the pipet with an appropriate
cleaning solution. (See the instructor for information)
2 Place approximately 500 mLs of distilled or deionized water in a clean beaker to
equilibrate to room temperature. Proceed with steps 3 and 4 while this equilibration
process takes place. After the water has equilibrated, measure the temperature of the
water to the nearest degree and look up the density of water at that temperature.
3. Practice filling a 5-mL volumetric pipet and adjusting the meniscus to the calibration
mark until you become proficient with the technique.
4. Weigh a clean, 125 mL plastic bottle and cap to the nearest ± 0.1mg.

5. Transfer 5.00 mL of the equilibrated distilled water to the plastic bottle using the
volumetric pipet (remember this type of pipet is ‘To Drain’.) Be careful and do not allow
the water to splash out of the container. Reweigh the bottle and cap plus water to the
nearest ± 0.1mg. Repeat as often as necessary; in other words, until your results
approximate the expectations of the manufacturer. (Note: It is not necessary to empty the
plastic bottle and cap between each addition. Just continue to add successive aliquots to
the bottle but be sure that you weigh the bottle and cap after each addition.) As in any
experiment, you should use the same balance throughout.

The 5-mL Eppendorf Pipet

You will follow essentially the same procedure as outlined above for the volumetric pipet. Of
course, you will not clean the device; it has replaceable and disposable tips. Your instructor will
describe and demonstrate the proper way to select the delivery volume, fill, and dispense liquid
samples.

The 50-m: Volumetric Flask

1. Weigh a clean, dry, 50-mL volumetric flask to the nearest ±0.1mg.

2, Transfer deionized water (used in part 1) to the volumetric flask until it is close to the
mark, then using a Pasteur pipet bring the liquid level up to the calibration mark.
Remember to ensure that the bottom of the meniscus is aligned with the calibration mark.

3. Carefully dry the flask and insert the top; weigh the flask and its contents on the
analytical balance.

4. Drain the liquid in the flask, refill and repeat the experiment as often as you must in order
to attain the published standards for 50-mL volumetric flasks.

CALCULATION OF RESULTS

Go to the literature and find the tolerance and precision associated with the volumetric ware used
in this experiment. Calculate the mean, standard deviation and confidence intervals for each of
your sets of data. Use suitable statistical tests to demonstrate that your results are or are not
consistent with expected precision and accuracy figures for your measuring devices. If your
results do not meet the literature values,; repeat the experiment until you are convinced that the
difference is real and not due to experimental error on your part.