Chem 223: Experiment 2

PRACTICE WITH BASIC TECHNIQUES

SAFETY FIRST!
BRING AND WEAR YOUR GOGGLES

(This experiment completely follows the lab: “Practice with basic techniques”. Chem 223. UIUC)

References: C, Chap. 2.
H4, H5 Chap. 2.
S & W, Chap. 19.
SWH, Chap. 30.

I. Purpose of the experiment

The Multi-technique Operations, Pipette Calibration and Weighing by Difference exercises
discussed on the following pages will introduce you to some basic operations you will need to
perform in later experiments. These simple measurement experiments give you practice in
pipetting, using the balance, and using your laboratory notebook. Careful attention to detail in this
experiment will inculcate good laboratory technique, which will be crucial in obtaining accurate
results in the later laboratories. Since a large fraction of your grade depends on accuracy, this lab
offers an important opportunity to practice. Think of it as spring training for analysts!

II. Before You Start the Lab

Review the Balance Tutorial before you come to lab!

When you arrive at the lab you will be assigned a lab bench and equipment locker, a
combination for your desk, and an equipment checklist. Check to see that you have all
the listed equipment and that it is not cracked, chipped or otherwise useless.

Become acquainted with safety devices, such as the showers. Sign and turn in a set of
laboratory regulations, if you have not already done so.

You will be given cards to fill out. Fill these out and return them.
You will be assigned to a balance. Meet the other people also assigned to that balance. It
is your responsibility to keep the balance clean - you will be penalized if you abuse
it. Each section will be given a demonstration on how to use the balance. You may
not use any balance other than the one to which you are assigned without the TA’s
permission.
You should scrupulously clean the equipment you need for next week with
detergent solution. Rinse with tap water and then three times with deionized
water. Cleaning solution should be used only if detergent solution does not do the
job. Go easy on the detergent. It does not take much.
Clean out your desiccators, if the desiccant appears wet or is clumped (or check
with TA). To open desiccator, slide the top off. Dump the old CaCl2 into the
specially marked container in the lab. If the desiccator looks dirty, clean it and dry
it well. Remove the old petroleum jelly with a paper towel. Grease on the inside may
require acetone for removal. Add only about two 50 mL beakers full of the desiccant
(CaCl2) to your desiccator. Regrease the rim and lid and remove any excess. Keep it
closed.
III. Multi-technique Operations
III.A. Quantitative Transfer
Using the top loading balance and a 50 mL beaker, weigh out about 2.5 g of either NaCl or KCl.
Add about 25 mL of deionized water.
Quantitatively transfer all of this solution to a 500.0 mL volumetric flask. This means that you
Figure 1. Quantitative transfer of
solution from a beaker to a
volumetric flask.
Figure 2. Stopcocks in the closed (left) and open
(right) positions.
Repeat the above experiment if you messed up the first time.
want to get all of the NaCl (or KCl) that you
put in the beaker into the volumetric flask. This
is accomplished as follows:
a. Insert a funnel into your 500.0 mL volumetric
flask.
b. Place a stirring rod on top of the beaker to guide
the liquid into the funnel as it is poured out of
the beaker.
c. Then using your polyethylene wash bottle,
(always filled with deionized water), rinse the
inside of the beaker, then the stirring rod, and
then the funnel itself such that all the rinse
water goes into the volumetric flask. This is
done with a lot of deionized water to insure
that
all the NaCl (or KCl) is transferred to the
volumetric flask and is not left behind, spilled
on the desk or otherwise lost.
d. Set the beaker with the stirring rod in it on the
desk and rinse what is on the tip of the funnel
into your volumetric flask.
Now, to check your technique, rinse the inside and
outside of the funnel, and the
stirring rod, and then the walls of
the beaker. Allow this rinse
solution to remain in the beaker.
Check your efficiency of transfer
now by adding one or two drops of
the 0.5 M AgNO3 solution (in a
small dark bottle that is in the lab)
to the beaker of rinse solution. DO
NOT add AgNO3 to the solution in
the volumetric flask. If the rinse
solution now turns white or cloudy,
your transfer was not quantitative.
Why does the formation of a cloudy
solution indicate incomplete
transfer?
 Figure 3. Rotating the burette to wet the interior surface. Figure 4. Reading the burette.

III.B. Practice using Burette.

Now, take the quantitatively transferred solution in the 500.0 mL volumetric flask, dilute to
volume with deionized water, and mix thoroughly. Practice using your burette with the solution in
your 500.0 mL flask:

Prime and fill the burette. To prime the burette, be sure the stopcock is closed, Fig.2.
Then pour 5 to 10 mL of the salt solution into the burette and rotate the burette (viz. Fig. 3)
to wet the walls. Allow the liquid to drain through the tip into a sink. Repeat this procedure,
and then fill the burette. Priming should be done with all delivering glassware before use.
Wait at least thirty seconds before taking an initial reading.
Take initial reading and all burette readings using a burette
reading card. Touch the card to the burette behind the
gradations. The top of the black stripe should be below the
meniscus so that the meniscus appears dark against the
white card, cf. Fig. 4.
Now let about 5 mL run into a 250 mL Erlenmeyer flask.
Wait at least 30 seconds and take the final reading. (The
amount of solution in the Erlenmeyer flask is equal to the
final reading minus the initial reading.) Write down the
final reading in your notebook, close it, and then ask a
neighbor or your friendly TA to take the final reading.
Compare the two readings. They should agree to within ± 0.01
mL. Do they? Notice the final digit in the burette reading is an
estimate of the distance between two lines. Always record two
decimal places from a burette reading.
Figure 5. Burette Repeat the previous steps of making initial and final burette
transferring solution to an readings two more times.
Erlenmeyer flask.

Refill the burette, and take a new initial reading. Now add 30 drops to the Erlenmeyer flask
with the burette, and take the final reading. Calculate the average volume of one drop.
Then repeat this, except with 40 drops and calculate the average volume of a drop. Record
these results and compare them. Now, practice adding "half-drops" to the flask. Record these
results for at least 10 half-drops, and calculate the average volume of your half-drops. In your
volumetric unknowns, you will want to try to get half-drop end points.

Dispose of the salt solution and clean up your equipment.

IV. 10.00 mL Pipette Calibration

This calibration is done by accurately weighing the volume of the liquid dispensed by the pipette. If the
density of the liquid is accurately known at the temperature at which you are working, the volume
dispensed can be accurately determined. Deionized water is the liquid you will use.

Figure 6. Filling a pipette Figure 7. Incorrect (left) and correct (right) methods of
with a mechanical suction releasing the pipette contents.
bulb.

Clean your 10.00 mL pipette so no droplets of deionized water are left on the inside surface as it
drains.
Weigh a 30 mL glass bottle and its cap to the nearest tenth of a milligram (0.0001 g)
on the analytical balance. Use finger cots to hold the bottle and manipulate the cap.
Fill the pipette to above the etched line with deionized water from a 250 mL beaker (note
the temperature of this water!). Use a filling bulb, viz. Fig. 6. Mouth pipetting is
forbidden! To use the suction bulb: (a) compress the bulb before you attach it to the
pipette, (b) place the compressed bulb over the end of the pipette and carefully release the
finger pressure to allow the liquid level to rise until it is somewhat above the
etched fill line, (c) rapidly remove the bulb and
simultaneously cover the end of the pipette with
the index finger of the hand holding the pipette,
cf. Fig. 7, (d) gently adjust the pressure on the
index finger to allow the liquid to fall until,
holding the pipette in a vertical position with
the etched line at eye level, the bottom of the
meniscus coincides with the etched line, (e)
touch the tip of the pipette to the side of the
beaker to remove any drop formed at the tip,
viz. Fig. 8. This manipulation is a bit tricky and
may have to be repeated several times until you
are sure you have it exactly right.
Figure 8. Removing the last drop of
liquid from a pipette by solid-solid Once this is accomplished, touch the pipette tip to
contact. the inside of the weighing bottle, and allow the
pipette to discharge its contents into the bottle. It
is best to allow the tip to touch the inner wall of
 the container near the bottom, but not in the liquid. Allow the pipette to drain by itself for
20 or 30 sec.. Do not blow out the remaining portion of water in the tip. Carefully remove
the pipette.
Note that the pipette is marked TD. What does this stand for? How would your procedure change if
your pipette were marked TC, instead?

Cover the bottle, and weigh the bottle and its contents.
This calibration should be done in triplicate and the three values should agree within 1 part
per thousand, i.e. 0.1%. There is no need to drain the water from the bottle; just use the final
mass of the last trial as your new initial mass for the next trial. Remember to keep the outside
of the bottle dry.
Common errors which you should be careful to avoid are: (a) warming the pipette by holding the
bulk portion in your hand, (b) failure to allow sufficient drainage time, (c) disturbing the liquid
that should remain in the tip (watch for air bubble formation!), (d) general carelessness in
handling the weighing container and top, (e) loss of water from the pipette as you move from eye
level to the weighing bottle (sudden movement will make some water squirt from the tip; slanting
the pipette a bit before moving it helps).
From the table of density vs. temperature, find the appropriate density and calculate the actual
volume your pipette holds.
Table 1. Density of Water Near 300K.
Temp. (°C) Density (g/mL) Temp. (°C) Density (g/mL)
20 0.99823 26 0.99681
21 0.99802 27 0.99654
22 0.99780 28 0.99626
23 0.99756 29 0.99597
24 0.99732 30 0.99567
25 0.99707

Obviously great care must be exercised in the manipulation of volumetric glassware. What should
you do in the following commonly encountered situations working with pipettes. (1) You notice a
small drop of liquid on the exterior surface of your pipette. (2) A small air bubble forms at the tip
of the pipette.
(3) After releasing the contents of the pipette into the receiving vessel you note that a small
drop remains on the interior surface of the pipette.

V. Weighing by Difference
Weighing by difference is both a simple concept and a simple laboratory task. However, if you
don't understand how to weigh by difference, you will do poorly on at least three labs. You
weigh by difference to avoid contaminating your precious sample. Use the data from this
section for error propagation for your lab report.
Fill a clean dry weighing bottle about one quarter full with NaCl (or KCl).1
Weigh the entire weighing bottle (top and bottom) and record the mass to 0.1 mg using
the analytical balance.
 Tap out about 0.8 g of solid into
your 250.0 mL volumetric flask.
Use a funnel.
Reweigh the entire weighing
bottle again.
Compute the change in mass. If
its change in mass is close to 0.8
g as desired, you are done. If not,
tap in some more powder and
reweigh until the difference is
Figure 9. (Left) Weighing bottle. (Right) about 0.8 g. If the mass added is
Proper handling of the weighing bottle. greater than 0.9 g, rinse your
volumetric flask well with
deionized water and start over.
When you are done, you have the initial and final masses, to four decimal places, of
the weighing bottle containing the powder. The difference is the mass of powder in the
volumetric flask.
Now that you’ve gone to all the trouble of weighing by difference, dilute the salt
solution and practice pipetting.
Dilute your NaCl or KCl in your 250.0 mL volumetric flask to volume with deionized
water and mix thoroughly.
Pour some of your salt solution into a beaker. If the beaker is wet, rinse with your
salt solution 3 times to insure that you do not dilute your salt solution.
Prime your 20.00 mL pipette by rinsing 3 times with the salt solution in the

beaker.

Pipette 20.00 mL of salt solution into a 250.0 mL Erlenmeyer flask. You can
dispose of the salt solution and clean up your glassware.

For this experiment only, you may dry the weigh bottle using a tissue. If you have time and
want to gain experience, use the ovens to dry to constant weight. This means the weigh bottle is
dried, cooled in a desiccator, and weighed. These three steps are repeated until nearly the same
mass is achieved twice in a row. In future experiments you must oven dry your weighing bottle.

FOR YOUR REPORT:

Calculate (1) volumes dispensed from burette, (2) average volume of a drop and half-drops, (3)
mean volume (in mL) of water transferred using 10.0 mL pipette from part II, (4) standard
deviation, relative percent error and relative standard deviation (in ppt) for 10.0 mL pipette
calibration, (5) concentration (in mg/mL) of NaCl (or KCl) solution from part III, (6) error
propagation.
Why is delivery glassware primed prior to use for quantitative transfer? Do volumetric flasks
need to be primed? Do volumetric flasks need to be dry before you use them? Explain.
PROBLEMS FOR EXTRA PRACTICE

1. Find the absolute uncertainty and percent relative uncertainty for each calculation.

Express the answers with the proper number of significant figures.

a. 6.2 (±0.2) - 4.1 (±0.1) b. 9.43 (±0.05) x 0.016 (±0.001)
c. 91.3 (±(1.0) x 40.3 (±0.2) / 21.1 (±0.2) d. [4.97 (±0.05) - 1.86 (±0.01)] / 21.1 (±0.2)

2. For the numbers 116.0, 97.9, 114.2, 106.8 and 108.3, find the mean, standard deviation, relative
standard deviation (in ppt), and 90% confidence interval for the mean.

3. What volume of 0.0110 M NaOH is required to completely titrate a 10.00 mL aliquot of a 0.0240 M
HCl?

4. If it takes 28.41 mL of 0.0510 M NaOH to titrate 20.00 mL of HCl, what is the concentration of the
HCl?

5. How many milliliters of 0.100 M KI are needed to react with 40.0 mL of 0.0400 M Hg2(NO3)2 if the
reaction is Hg22+ + 2I-  Hg2I2(s)?
6. A cyanide solution with a volume of 12.73 mL was treated with 25.00 mL of Ni2+ solution
(containing excess Ni2+) to convert the cyanide to tetracyanonickelate(II):
4CN- + Ni2+  Ni(CN)42-
The excess Ni2+ was then titrated with 10.15 mL of 0.01307 M ethylenediaminetetraacetic
acid (EDTA). One mole of this reagent reacts with 1 mol of Ni2+:
Ni2+ + EDTA4-  Ni(EDTA)2-
Ni(CN)42- does not react with EDTA. If 39.35 mL of the 0.01307 M EDTA was required to
react with 30.10 mL of the original Ni2+ solution, calculate the molarity of CN- in the 12.73
mL cyanide sample.