Basic Tools and Operations of

Analytical Chemistry
Tools in Heating, Evaporating, Solvent Removal and Refluxing
Liquids
Open-Dish Evaporation

Evaporating dish
 Florence Flasks

Evaporating dish Florence Flasks

3. hot plate
Used for heating substances and liquids in beakers and flasks.
Water baths
• heated on a hotplate, are
most commonly used to heat
solutions to 100o C-100oC
(boiling baths).
 Boiling water bath Water bath to cool an apparatus
Heating a flask with a sand Allowing a flask to cool.
bath.
Oil baths are much like water baths, but use silicone or mineral
oils in order to enable temperatures hotter than the boiling point
of water (> 100oC100oC)

It is also quite common for the oil to be electrically heated,

through immersion of a coiled wire connected to a "Variac"
(light blue piece of equipment)
wire gauze
Used with a ring clamp to
support glassware over a
Bunsen burner. Spreads
flame out for more even
heating.

striker
 Used to light a gas
burner. crucible tong

Used to hold crucibles and

evaporating dishes when they are
hot.
Reflux
apparatus
Reflux apparatus, with
arrows indicating the
direction of water flow,
b) Reflux diagram
c) Incorrect clamping of
a reflux apparatus.

A reflux setup
allows for liquid to boil and condense, with the condensed liquid
returning to the original flask. A reflux setup is analogous to a distillation,
 with the main difference being the vertical placement of the condenser.
The liquid remains at the boiling point of the solvent (or solution) during
active reflux.
Step-by-Step Procedures

a) Pouring in solution, b) Reaction using a stir bar (solution is colorless),

c+d) Same reaction using boiling stones.
Using a sandbath
 a. Filling a heating mantle
with sand to ensure a
perfect fit
b. Heating a reflux
apparatus with a sand
bath.

c. Do not turn off the water

flowing through the
condenser until the
solution is only warm to
the touch.

After a few minutes of air

cooling, the round
bottomed flask can be
immersed in a tap water
bath to accelerate the
cooling process
Reduced-Pressure Evaporation
• Evaporation can be accomplished from a solution quickly by placing
it in a side-arm flask, sealing the flask, and then applying vacuum.
Rotary Evaporator
• remove liquids from preparations that need to be dry.
• prepare samples for analysis.
 Rot
ary Evaporators
A piece of apparatus consisting of a motor unit that rotates
the evaporation flask, a vacuum system, a heated water
bath and a condenser, which is used to remove solvents
from samples under reduced pressure.
Distillation

• Simple distillation can be

used to remove solvent.

• It works well if the

solution is composed of
a solid and a low-
boiling solvent, or if
the solution is
composed of a high
boiling liquid and a low
boiling solvent (BP
differences >100°).
Steam Distillation

Steam distillation is used to distil compounds at a

temperature lower than the normal boiling point. The desired
material distilled at a temperature of fewer than 100 OC
 Major conditions are observed
to
use steam distillation:

1.Extraction of temperature
sensitive compounds
2.When material to be
extracted is
immiscible
3.When substance is
chemically
non reactive with water.
Fractional Distillation
• process by which components
in a chemical mixture are
separated into different parts
(called fractions) according to
their different boiling points.

Use for filtering non-gelatinous precipitates.

 Fig. 2.21. Filtering crucibles: (a) Gooch crucible;
(b) sintered-glass crucible; (c) porcelain
filter crucible.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

Beaker
Used to hold, mix, and heat
liquids.

Test Tube
Used to hold and mix
liquids.

Test Tube Clamp

Used to hold a test tube,
particularly when hot.

Test Tube Rack

Used to hold several test
tubes at one time.
Used to dry samples before weighing.
Usually 110o C used.
 Fig. 2.18. Drying oven.
©Gary Christian, Analytical Chemistry, 6th Ed.
(Wiley)
 Measuring Mass

Types of Analytical Balances

An analytical balance is
a
weighing instrument
with a
maximum capacity that
ranges
from 1 g to a few kg
with a
precision of at least 1
part in
105 at maximum
capacity.

Macrobalances have a
maximum capacity ranging
between 160 - 200 g;
measurement can be made
with a standard deviation of
±0.1mg.
Types of Analytical Balances
Semimicroanalytical balances have a
maximum load of 10 - 30 g with a precision
of ±0.01mg.

Microanalytical balance has a capacity of 1

-3 g and a precision of ±0.001mg.
Modern balances are electronic. They still compare one mass against another since
they are calibrated with a known mass. Common balances are sensitive to 0.1 mg.
 Fig. 2.1. Electronic analytical balance.
©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)

Electronic balances operate on the principle of

emf compensation – the
hanger
compensation current to bring the pan back to
its original position is
proportional to the sample weight.

position
 scanner

coil
temperature sensor
©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley) ©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)

Fig. 2.2. Operating principle of electronic Mechanical balances operate as first class
levers. M1L1 = M2L2
balance.
 Fig. 2.3. Principle of analytical balance.

The single pan balance operates by removing weights equal to the mass of the sample.
Small residual imbalances are read optically from the deflection of the beam.
 Fig. 2.4. Schematic diagram of a typical single-pan balance.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

The single-pan balance is as accurate as ©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)

electronic balances, and almost as fast.

But it can’t be interfaced to a computer to
collect and process data.
And you have to read a scale instead of a
digital number.
 2.5. Typical single-pan balance.

Fig.

Desiccators and Desiccants

• Oven drying is the most common way of

removing moisture from solids.
 • This approach is not appropriate for
substances that decompose or for those from
which water is not removed at the
temperature of the oven.
Weighing bottles are used for drying samples. Hygroscopic samples are weighed by
difference, keeping the bottle capped except when removing the sample.

Fig. 2.6. Weighing bottles.

©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)

A weighing dish or boat is used for direct weighing of samples.

Fig. 2.7. Weighing dish.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

Desiccators and Desiccants

• Dried material are stored in desiccator while

they cool so as to minimize the uptake of
 moisture.

• The base section of the desiccator contains a

chemical drying agent (desiccants) such as
anhydrous calcium chloride, calcium sulfate,
magnesium perchlorate or phosphorus
pentoxide.
 D

esiccator
CaCl2 is commonly used.
It needs periodic replacement when wet or caked.
©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)

Factors that affect readings on analytical

balances:

•Temperature
•Vibrations
•Air drafts
•Chemical reactions
•Uncalibrated scales
•Magnets
•User error
•Improper grounding
•Slope
•Inappropriate handling of the
sample
Five precautions for accurate sample

weighing: 1. Keep the

balance calibrated

• The scales’ calibration must

be
validated as per the
requirements of a
recognized
national calibration laboratory.
Keep the balance calibrated
using the standard calibration
procedures against daily, weekly,
and monthly schedules.

• Never touch the standard

 weights with your hands.
Five precautions for accurate sample

weighing: 2. Ensure appropriate environment

• Check the horizontal positioning of

the
balance.
• Keep the balance in a vibration-free
environment.
• Ensure that you place the balances
in an area with controlled humidity
and
temperature.
• They should not be exposed to weighing chamber.
direct sunlight since it can cause Thermohygrometer
temperature variations inside the
Five precautions for accurate sample
 weighing: 2. Ensure appropriate environment

• Don’t place the balances next to doors

or windows since opening or closing
them will result in air drafts. This
could affect the weighing process.

• Ensure that you weigh the samples

only after closing the weighing chamber
doors.

• Keep the weighing chamber clean to

prevent cross-contamination of samples
and erroneous readings.
Five precautions for accurate sample weighing:
3. Handle the weights properly
• Never touch the weights with bare
hands. Hand grease can cause
errors
in the readings. Use a pair of
clean
forceps while placing the
samples.
• Use wooden tweezers or tweezers
covered with rubber on the
tips to
prevent the weights from
getting
scratched. Use gloves when
handling heavy weights.
4. Store the weights in the
right manner
 • Always store the weights in a room free of
moisture, corrosive gases, and dust. If the weights
get rusted or dust sticks to them, the mass of the
weights will increase. This will result in inaccurate
readings.

• After using the weights, place them inside a

desiccator to keep them dry
5. Take the right measures
to weigh the samples

• Use a clean spatula of

appropriate size while placing
the sample.

• Weigh the sample quantity in a

a flask rather than opting for
butter paper weighing. The
 latter can introduce errors.

• Before you record the

readings,
allow them to stabilize.
Correcting Mass for the
Buoyancy of Air

Because of the buoyancy of air, an object always weighs

less in air than it does in a vacuum.

Correction for buoyancy

Wv- object’s true weight in vacuo
Wa- weight in air

Do - object’s density
Dw -density of the calibration weight, and 0.0012 -
density of air under normal laboratory conditions
 (densities in units of g/cm3).

The greater the difference between Do and Dw the more

serious the error in the object’s measured weight.
Example:

A 10-mL volumetric pipet was calibrated using a balance calibrated with brass
weights having a density of 8.40 g/cm3. At 25 oC the pipet dispensed 9.9736 g of
water. What is the actual volume dispensed by the pipet and what is the
determinate error in this volume if we ignore the buoyancy correction? At 25 oC
the density of water is 0.997 05 g/cm3.

Solution
actual volume of
water dispensed
by the pipet

If buoyancy correction is
ignored, the pipet’s volume
is
 negative determinate error = -0.11%.
2.6 Filtration and Ignition of
Solids
Use a desiccator to cool a dried or ignited sample.
Cool a red hot vessel before placing in the desiccator.
Do not stopper a hot weighing bottlle (creates a partial vacuum on cooling).

Fi
g. 2.16. Desiccator and desiccator plate.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
Crucible
Used for holding chemicals
during heating to very high
temperatures.

Crucible Tongs
Used to hold crucibles.

Clay Triangle
Used to support a crucible
during heating.
Used to ignite samples at high temperatures, e.g., to dry ash organic matter.
 Fig. 2.17. Muffle furnace.
©Gary Christian, Analytical Chemistry, 6th Ed.
(Wiley)
Measuring Volume

Volume Measurement
Volumetric flasks are calibrated to contain an
accurate volume. See the inside back cover of
the text for tolerances of Class A volumetric
glassware.
Graduated Cylinder
Used to measure a
precise volume of a
liquid.
©Gary Christian, Analytical Chemistry, 6 th Ed. (Wiley)
Fig. 2.8. Volumetric flask.
Volumetric pipets accurately deliver a fixed volume.
A small volume remains in the tip.

Fig. 2.9. Transfer or volumetric pipets.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

Measuring pipets are straight-bore pipets marked at different volumes.

They are less accurate than volumetric pipets.
 Fig. 2.10. Measuring pipets.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

Syringe pipets precisely deliver microliter volumes.

They are commonly used to introduce samples into a gas chromatograph.
 Fig. 2.11. Hamilton microliter syringe.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

These syringe pipets can reproducibly deliver a selected volume. They

come in fixed and variable volumes. The plastic tips are disposable.
 Fig. 2.12 Single-channel and multichannel digital
displacement pipets and microwell plates.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
 ©Gary Christian,

Analytical Chemistry, 6th Ed. (Wiley)

These accuracies and precisions are typical for single channel pipets. ©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
A 50-mL buret is marked in 0.1 mL increments. You
interpolate to 0.01 mL, good to about ±0.02 mL. Two
readings are taken for every volume measurement.

Fig. 2.13. Typical buret.

©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)

Position the black field just below the meniscus.

Avoid parallax error by reading at eye level.
 Fig. 2.14. Meniscus illuminator.
©Gary Christian, Analytical Chemistry, 6th Ed. (Wiley)
©Gary Christian,
Place the flask on a white background.
Place the buret tip in the neck of the flask while your swirl.

Fig. 2.15. Proper technique for titration.

Analytical Chemistry,
 6th Ed. (Wiley)

Pipets
• Pipette Calibration and Pipetting Accuracy

Pipette - a high precision laboratory

instruments that requires proper maintenance
on a regular basis.
Pipette Storage – Where and How for Pipetting
Accuracy

Proper storage -very important factor in maintaining

an accurate pipetting result.

• Upright –prevent any liquids from corroding the

 internal workings of your pipette.

• Environmental Factors – Store your pipettes away

from the window, heating sources and in an
environment with low moisture
Ways to Stop Pipetting Errors
From Ruining Your Experiments
.
Without accurate pipetting

• experiments would not be reproducible

• stock solutions would be inaccurate
• assays would have such large errors that comparing
them would be meaningless.

Know How Pipets Work!!!

 Precision instruments they may be, but the accuracy of
your micropipettes depends on you
Air Displacement Pipette
• works a bit like a syringe, except that there is an air-filled
cushion between the piston and the sample.
Limitations:
• Temperature and pressure affects the volume
of the air cushion, which affects pipetting
accuracy.
• volatile solvents can evaporate
into the air
cushion, which leads to an inaccurate
and
lower dispensed volume than what is
displayed on the pipette.
• barrel of air displacement pipettes is
vulnerable to
contamination by the pipetted
solution, corrosives or bio-hazardous
material, this can be a problem.
Positive displacement pipettes
• also work like
a
syringe, but
they
don’t have an
air
cushion—
unlike air
displacement
pipettes.
• more accurate
for
pipetting
volatile
 solvents because
there is no place (air
cushion) for the
solvent to evaporate.

The lack of air cushion decreases the chance of contamination when pipetting
corrosives and bio-hazardous material, which makes positive displacement
pipettes more suitable to working with those reagents.