Exercise No.

2 Basic Operations of Analytical Chemistry

Exercise No. 2
BASIC OPERATIONS OF ANALYTICAL
CHEMISTRY

Objectives

1. To know the basic operation of analytical balance

2. To be able to measure substances quantitatively using an analytical balance.
3. To know the proper techniques in transferring solutions.
4. To measure an aliquot and prepare solution from an aliquot.
5. To calibrate a pipette.
6. To know the proper use of burette.

Reagents

Tablets
Solid KMnO4
Distilled water

Apparatus

Analytical balance
50-mL beaker
100-mL volumetric flask
200-mL volumetric flask
glass funnel
stirring rod
wash bottle
10-mL pipette
suction bulb
Erlenmeyer flask
400-mL beaker
Cork stopper
Thermometer
burette
burette clamp
iron stand

Page 1 of 7 Exercise 2 CM124-1L

Exercise No. 2 Basic Operations of Analytical Chemistry

Procedure

I. Use of Analytical Balance

A. Check the analytical balance and ensure that there are no foreign materials in
the pan.
B. Zero-in the balance by using the “tare button”.
C. Randomly collect 5 tablets from the bottle. Keep track of the identity of the tablet
by placing it in a piece of paper with label. Be careful not to touch the tablets with
your bare hands, use tweezers in handling it.
D. Using a sample pan weigh each tablet and record the mass on your notebook.
(Note: make sure to set the analytical balance to zero before placing the tablet on
the sample pan)
E. Set the balance again to zero, this time place all the five tablets and record the
total mass.
F. Remove each tablet (keep track the identity) one at a time and record each
reading. Determine the mass of each tablet removed by difference and record it
on your notebook.

Additional information about Proper Handling of Analytical Balance

The correct weighing procedure depends somewhat on the design of the balance. Most
single pan analytical balances have a knife edge supported fulcrum. Such balances are
always equipped with a pan release lever which raises and lowers the fulcrum off of a
finely-machined knife edge. In the Environmental Engineering Teaching Laboratory we
have a Mettler H80 which employs a taught band fulcrum support system, rather than a
knife edge. It, therefore, does not require a pan release. The Mettler H80 is pictured on
the following page. The numbers refer to the following:

1. Level indicator 8. Zero adjustment knob

2. Weight control knob for 10 9. Readout
g increments
3. Weight control knob for 1 g 10. Micrometer knob
increments
4. Power switch for optical 11. Image definition
scale adjustment
5. Weighing pan 12. Cover plate of lighting
system
6. Leveling feet 13. Power cable
7. Sliding door, right 14. Sliding door, left

Page 2 of 7 Exercise 2 CM124-1L

Exercise No. 2 Basic Operations of Analytical Chemistry

Exterior of the Mettler H80 Analytical Balance

Some general rules should be kept in mind when using an analytical balance:

1. Allow samples to reach room temperature before weighing. Samples that are too hot
will set up convection currents and the apparent sample weight will be incorrect. A
slowly drifting apparent sample weight is indicative of this problem.

2. Chemicals should be placed in a weighing bottle, a plastic weighing tray, or coated

weighing paper. Weighing paper is best for small quantities (usually <1g); weighing
trays are used for larger amounts; and stoppered weighing bottles are recommended for
reactive, volatile, toxic or hygroscopic substances. In the absence of a weighing bottle,
a small beaker and watch glass may be substituted. Never place chemicals directly on
the pan!

3. The analytical balance should be kept clean at all times. If a solid is spilled inside the
weighing chamber, carefully remove it with the balance brush. The desiccant should be
replaced or regenerated when it changes color. Used weighing papers and trays should
be immediately discarded.

Page 3 of 7 Exercise 2 CM124-1L

Exercise No. 2 Basic Operations of Analytical Chemistry

The procedure for weighing with the Mettler H80 is as follows:

1. Insure that the balance is level by verifying that the air bubble is in the center of the
circular marking of the level indicator (1).

2. Verify that the weight control knobs (2,3) and micrometer knob (10) are in the zero
position.

3. Carefully clean off the pan (5) with the soft brush provided.

4. Actuate power switch (4). Optical scale image appears.

5. Close both doors and adjust zero point, if necessary, with the zero adjustment knob
(8).

6. Open one door and place the empty weighing vessel on the center of the pan. Its
weight is referred to as the "tare", and the process of weighing it is called "taring".
Objects to be weighed may be moved by hand prior to determination of the tare and
after final weighing only. Should the sample container need to be moved between taring
and final weighing, use either clean, dry rubber gloves (not latex), tongs, or a paper
loop. Fingerprints will add significant mass to small samples.

7. Close the glass doors tightly to avoid unsettling air currents.

8. Turn weight control knob (2) until optical scale image moves through readout field,
the turn knob (2) back one step.

9. Turn weight control knob (3) until optical scale moves into readout field.

10. Turn micrometer knob (10) until next scale division line is exactly in center of index
fork.

Figure 15.3: Mettler H80 Readout

11. Read weight.

12. Open door and remove object from pan.

13. Return weight control knobs (2,3) and micrometer knob (10) to zero, and brush off
pan and weighing chamber, if necessary.

Page 4 of 7 Exercise 2 CM124-1L

 Exercise No. 2 Basic Operations of Analytical Chemistry

14. Repeat steps 3-13 for weighing vessel plus sample.

Technique for Handling a Weighing Bottle with a Paper Loop

II. Quantitative Transfers

A. Measure 0.400 g of KMnO4 using a 50-mL beaker as the sample pan. Make sure
to press the tare button before placing KMnO4. Do not return any excess
chemical in the reagent bottle.
B. Dissolve the KMnO4 with 20.0 mL of distilled water. Stir gently to avoid any loss.
C. Transfer the solution to a 100-mL volumetric flask fitted with a small funnel. To
avoid spilling, use a stirring rod in transferring the solution. To remove the last
drop, place the stirring rod on the sprout of the beaker. Wash the remaining
potassium permanganate in the beaker by adding more water to the beaker, stir
and transfer it again in the volumetric flask following the same procedure. Repeat
this washing until no trace of the color of potassium permanganate remains.
Record the number of washings made.
D. Rinse the stirring rod, allowing the rinse water to flow into the volumetric flask.
Finally rinse the funnel and remove it from the flask. Use the wash bottle in
rinsing.
E. Dilute the solution in the volumetric flask to the mark (lower meniscus must be on
the mark measured at eye level).
F. Stopper the flask. Shake the solution by making several inversions (about 10
times) allowing the bubbles to reside on the top of the neck before making
another inversion.
G. Compute the concentration of the solution made.

III. Measurement of an Aliquot and Dilution

A. Carefully fill the pipette to a level somewhat above 10.0 mL of the potassium
permangate solution you prepared. Make certain there are no bubbles in the bulk
of the liquid or foam at the surface. Tilt the pipette slightly from the vertical and
wipe the exterior free of adhering liquid. Touch the tip of the pipette to the wall of

Page 5 of 7 Exercise 2 CM124-1L

 Exercise No. 2 Basic Operations of Analytical Chemistry

the volumetric flask and slowly allow the liquid level to drop by partially releasing
the forefinger. Halt further flow as the bottom of the meniscus coincides exactly
at 10.0 mL.
B. Place the pipette tip well a 200-mL volumetric flask, and allow the liquid to drain.
When free flow ceases, rest the tip against the inner wall of the flask for 10
seconds. Finally withdraw the pipette with a rotating motion to remove any liquid
adhering to the tip. (Note: the small volume remaining inside the tip of the pipette
should not be blown or rinsed into the flask)
C. Dilute the solution in the volumetric flask to the mark (lower meniscus must be on
the mark measured at eye level).
D. Stopper the flask. Shake the solution by making several inversions (about 10
times) allowing the bubbles to reside on the top of the neck before making
another inversion.
E. Compute the new concentration of the solution made.

IV. Calibration of Pipette

A. Clean a 10-mL pipette. When a pipette, burette, or another piece of volumetric
glassware is cleaned properly, no droplets of reagent remain on the internal
surfaces when they are drained. This is very important for accurate and
reproducible results. If the reagent adheres to the inside of a pipette, the nominal
volume of the pipette cannot be delivered.
B. Obtain a 400-mL beaker of distilled water equilibrated to room temperature.
C. Determine the mass of the flask and the stopper and record it to the nearest 0.1
mg.
NOTE: Do not touch the flask after the weighing. Use tongs or a folded strip of
waxed paper to manipulate the flask.
D. Measure and record the temperature of the water.
E. Pipette 5 mL of distilled water to the flask. Stopper the flask, record the mass of
the flask and the water and determine the mass of the 5 mL water.
F. In the same way, add a second 5 mL of water to the flask. Replace the stopper,
and once again record the mass of the flask and the water and determine the
mass of the 10 mL water.
G. Repeat this process until you have determined four consecutive masses of water
that agree within a range of 0.02 g.
NOTE: If the determinations of masses of water delivered by the pipette do not
agree within this range, the pipetting technique may be wrong.
H. Correct the mass for buoyancy and calculate the volume of the pipette in
milliliters.
Volume = mass of water in grams x factor

Page 6 of 7 Exercise 2 CM124-1L

Exercise No. 2 Basic Operations of Analytical Chemistry

Table 1. Volume occupied by 1.00 g of water weighed in air against stainless

steel weights
Volume, mL Volume, mL
Temperature, Temperature,
T (0C) Corrected T (0C) Corrected
at T at T
to 200C to 200C
10 1.0013 1.0016 21 1.0030 1.0030
11 1.0014 1.0016 22 1.0033 1.0032
12 1.0015 1.0017 23 1.0035 1.0034
13 1.0016 1.0018 24 1.0037 1.0036
14 1.0018 1.0019 25 1.0040 1.0037
15 1.0019 1.0020 26 1.0043 1.0041
16 1.0021 1.0022 27 1.0045 1.0043
17 1.0022 1.0023 28 1.0048 1.0046
18 1.0024 1.0025 29 1.0051 1.0048
19 1.0026 1.0026 30 1.0054 1.0052
20 1.0028 1.0028

V. Reading and Using a Burette

A. Mount a burette on a burette clamp and fill it up with distilled water.
B. Get the initial reading of the volume of water after 30 seconds. Use a burette
reading card to take the readings. Never adjust the volume of the solution in a
burette to an exact 0.00 mL. Attempting to do so will cause inaccuracy in the
measurement process and will waste time.
NOTE: A burette reading card can be easily prepared by attaching a piece of
black electrical tape to a 3” x 5” index card.
C. Allow about 5 mL run into a 250-mL Erlenmeyer flask. Wait at least 30 seconds
and then take the “final reading.” The amount of solution in the Erlenmeyer flask
is equal to the difference between the final reading and the initial reading. Notice
that the final digit in the burette reading is your estimate of the distance between
two consecutive 0.1-mL marks on the burette.
D. Refill the burette, and take a new zero reading. Add 30 drops to the Erlenmeyer
flask, and take the final reading. Calculate the mean volume of one drop; repeat
this using 40 drops, and again calculate the mean volume of a drop. Record
these results and compare them.
E. Finally, practice adding half-drops to the flask. Calculate the mean volume of
several half-drops, and compare your results with those obtained with full drops.
In performing titrations, you should attempt to determine end points to within half
a drop to achieve precision.

Page 7 of 7 Exercise 2 CM124-1L