Contents

1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

LABORATORY APPARATUS

What are the lab apparatus you have used?

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LABORATORY APPARATUS

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LABORATORY APPARATUS

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DESSICATORS

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WEIGHING BOTTLES
Weighing bottle are
used for drying
samples.
Hygroscopic samples
are weighed by
differences, keeping
the bottle capped
except when removing
the sample

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

ANALYTICAL BALANCE
An analytical balance is an instrument that is
used to obtain 4 to 5 digits to the right of
decimal point.
All analytical balances require a wind screen
or cabinet in order to realize the required
precision of the measurements.
Measure mass to a very high degree of
precision (0.1 or 0.01 mg)

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TYPES OF BALANCES

Single pan analytical

mechanical balance

Balances

Auxillary balance
(Top pan balance)

Electronic analytical
balance

10

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ANALYTICAL BALANCE

A weighing boat or dish is used for direct

weighing of samples.

11

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PLACEMENT OF ANALYTICAL BALANCE

Explain what is wrong of this situation?

12

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PLACEMENT OF ANALYTICAL BALANCE

The balance should not be placed near an open

window or directly in front of the air-condition
air vent. This will cause draft.

13

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PLACEMENT OF ANALYTICAL BALANCE

Explain what is wrong with this situation

The balance should have a stable support, usually

a concrete bench.
14

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PLACEMENT OF ANALYTICAL BALANCE

Explain what is wrong with this situation

The balance should not be placed where there is

direct sunlight.
15

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PLACEMENT OF ANALYTICAL BALANCE

Explain what is wrong with this situation

The room temperature is too high. The room

should be air-conditioned.
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PLACEMENT OF ANALYTICAL BALANCE

Stability
Temperature and evaporation
Far from drafts (movement of air)

CARE & USES

Always handle the analytical balance with great
care. Never drop it!
Keep clean.

17

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

GENERAL RULES FOR WEIGHING

The balance should be warmed up for at least half an hour

before use.
Before turning on, ensure all the doors are closed and the pan is
not touching the draft ring.
Never handle objects to be weighed with fingers. Use tongs or
finger pads (gloves) to prevent uptake of moisture by dried
objects.
Centre the substance to be weighed in the middle of the pan.
Weigh at room temperature.
Never place chemicals directly on the pan, but weigh them in a
vessel (dish, boat, weighing bottle, small beaker)
Always brush spilled chemicals off immediately with a soft brush.
Always close the balance case door before making the weighing.
Air currents will cause the balance to be unsteady.

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USE OF THE ANALYTICAL BALANCE

Press the TARE on the balance to zero the display.
Place a sheet of quantitative filter paper on the
pan of the balance.
Use a clean, dry spatula to carefully measure the
required quantity of solute calculated.
Read the display weight after the display is stable,
indicated by the no-motion symbol switches on or
off.
Record the weight of the solute for reference.

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WEIGHING OF SOLIDS
DIRECT WEIGHING
A weighing
dish/bottle/boat is
used.
The dish is weighed
empty and then with
the sample.
Direct weighing is
satisfactory only if the
sample is nonhygroscopic.

WEIGHING BY DIFFERENCE

Solid chemical materials

are usually weighed and
dried in a weighing bottle.
Replicate weighings are
most conveniently carried
out by weighing the
difference.
Also if the sample is
hygroscopic, weighing by
difference with the bottle
capped must be
employed.
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TECHNIQUE OF WEIGHING BY DIFFERENCE

The sample in the weighing bottle is weighed,
and then a portion is removed and
quantitaively transferred to a vesel.
Then the weighing bottle and the sample is reweighed, and from the difference in weight, the
weight of sample is calculated.
The next sample is transferred and the weight
is repeated to get its weight by difference, and
so on.

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WEIGHING OF LIQUIDS OR SOLUTION

WEIGHING BY DIFFERENCE
DIRECT WEIGHING
The liquid is
By pipetting out an
aliquot from the
transferred to a
weighing bottle, the
weighing vessel (e,g,
inside of the pipette
a weighing bottle)
must be rinsed several
times after transferring.
which is capped to
Care should be taken
prevent evaporation
not to lose any sample
during the weighing,
from the tip of the
and then weighed.
pipette during
transferring.

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ERROR IN WEIGHING

Weighing in the c=vacuum is the most accurate.

The weighings are made on a balance will, of course, give the
weight in air. When an object displaces its volume in air, it will
buoyed up by the weight of air displaced. (Archimedes
principle)
Actually in most cases, a correction is not b=necessary
because the error resulting from buoyancy will cancel out in
percent composition calculation.
The same error will occur in the numerator (as the
concentration of a standard solution or weight of a gravimetric
precipitate) and in the denominator (as the weighed sample)
Of course, all weighing must be made with materials in the
same type of container (same density) to keep the error
constant.
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CORRECTION FOR BUOYANCY

A buoyancy error will affect data if the density
of the object being weighed differ significantly
from that of the standard weight.
This error has its origin in the difference in the
buoyant force exerted by the medium (air) on
the objects and on the weights.
Weight of object in air can be corrected to the
weight in vacuum by:

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CORRECTION FOR BUOYANCY

Wvac = Wair + Wair [ 0.0012/Do 0.0012/Dw]

Wvac = weight in vacuum/corrected mass of the

object, g
Wair = observed weight in air, g
Do = density of object
Dw = density of weight
0.0012 = density of air

26

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EXAMPLE

A bottle of weighed 7.6500 g empty and 9.9700 g

after filling an organic liquid with a density 0.92
gcm-3. The balance was equipped with stainless
steel weights (d = 8.0 gm-3). Calculate the
corrected mass of the organic liquid sample.

Observed weight in air, Wair = (9.9700 7.6500) g

= 2.3200 g
W vac/corr = 2.3200 + 2.3200 [ 0.0012/0.92o
0.0012/8.0w] = 2.3227 g

27

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A 20 mL pipet is to be calibrated. A stoppered

flask when empty weighs 29.2780 g. Water is
delivered into it from the pipet, and it now
weighs 49.2720 g. If stainless steel weights are
used, calculate the corrected weight of water
delivered.

Given: density of air = 0.0012 g/mL

Density of stainless steel weights = 8.0 g/mL

28

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

VOLUMETRIC GLASSWARE

1. For very accurate volumetric analysis you need to

calibrate the volumetric glassware.
2. All volumetric glasswares are allowed tolerance by
manufacturer.
For example, a volumetric pipette may be labeled 25
mL, but it will deliver that volume with a tolerance. A
100 mL volumetric flask is manufactured to a tolerance
of 0.08 mL and since liquids and glass expand or
contract as temperature rises and falls, the tolerance
applies at the temperature indicated on the flask,
usually 20 C.
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MEASURING VOLUME
The unit of volume is liter (L)
It is defined as one cubic decimeter (dm3)
Milliter (ml) is one thousand of a liter
1 liter = 1000 ml

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Glassware

Volumetric

TD
(To deliver)
-pipette, buret

TC
(To contain)
- Volumetric flask,
pipette, graduated
cylinder

Non
volumetric

TC
(To contain)
-Beaker, flask

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Glassware

TC
Volumetric
flask
(For preparation
of standard
solution)

Volumetric

Graduated
Cylinder
(For rapid
measurement of
liquid volume,
semi-accurate
liquid measuring
vessel)

Pipette
(For
transferring
liquid
between
containers)

TD
Burette
(For titration,
accurate in
dispensing
aliquots of
solutions)
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Glassware

Non Volumetric

TC
Beaker
(For transferring
liquid to another
container)

Flask
(For containing a
certain volume)
34

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PIPETTE
Pipette is used to transfer a
particular volume of solution.
It permits the transfer of
accurately known volumes
from one container to
another
It is sometimes used to
deliver a certain fraction or
portion (aliquot) of a solution

35

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TYPES OF PIPETTES

Volumetric
Measuring
Mohr
Serological

36

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TWO COMMON TYPES OF PIPETTES

Volumetric or transfer pipette
(bulb pipette) (TD)

Measuring or graduated pipette

(clinical, Mohr or serological pipette
(TC)

Sizes of 100
mL to 5 mL
or less)

The measuring
pipettes range
from total volume
of 25 mL to 0.1
mL.

37

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Pipettes are calibrated to deliver (TD) or to contain (TC)

If the pipette were calibrated TC, the small remaining volume
should be shaken or blown out to obtain the correct amount of
material

If the volume pipettes are calibrated to deliver (TD), a certain

small volume remaining in the tip. This should not be shaken or
blown out.

In delivering , the pipette is held vertically and the tip is

touched on the side of the vessel to allow smooth delivery
without splashing and so that the proper volume will be left in
the tip.
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VOLUMETRIC PIPETTES
Used for accurate measurements, since it is
designed to deliver only one volume and is
calibrated at that volume.
Should be used when accuracy and
reproducibility are crucial, because these can
achieve accuracy to four significant figures.

39

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SPECIFICATIONS ON VOLUMETRIC PIPETTE

On a volumetric pipette, the specifications

indicate
How

much liquid will be transferred if the liquid is

drawn up to the calibration line on the neck
The temperature at which the calibration was made
Whether is a TD or TC pipette

40

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TD VOLUMETRIC PIPETTE

The volumetric pipette (a bulb shaped) is used

for accurate measurements since it is designed
to deliver only one volume and is calibrated at
that volume. Volumetric pipetts are available in
sizes of 100 mL to 0.5 mL or less.

Pipette
capacity
(mL)
Tolerea
m=nce
(mL)

0.01

10

0.04

25

0.06

50

0.08

100

0.12

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MEASURING PIPETTES
They are straight glass or plastic tubes with one
tapering end.
Calibrated into small divisions so that various
amounts of liquid can be measured with the same
pipet.
Usually used to measure any amount between 0.1
mL and 25.0 mL.
They are not as accurate due to the fact that any
imperfection in their internal diameter will have a
greater effect on the volume delivered.

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MEASURING PIPETTES

MOHR
- The graduations on these always
end before the tip

SEROLOGICAL
- The graduation continues to the tip
If a serological pipette has a frosted
band or two thin rings around the
neck, then it is a blow-out pipette.

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SPECIFICATIONS ON A MEASURING PIPETTE

Printed on the neck of the pipette are:

The

maximum volume of the liquid that can be

transferred
The size of the divisions on the pipette.
The temperature at which calibrations were made
If the pipette is a to deliver (TD) or to contain
(TC)

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BASIC TECHNIQUES FOR USING PIPETTE

Clean the pipette with detergent and water.

Rinse thoroughly, first with tap water then with Distilled water.
Rinse with the intended solution, twice.
Using a filler, fill the pipette and adjusting the meniscus to the
calibration mark. At the top of a pipette is an etched ring. Fluid must
be drawn up above a ring indicating the volume and then released
slowly until the bottom of the meniscus is exactly at the ring.
Hold vertically, allow water to run out with the tip of the pipet
touching the side of the receiving flask, being careful that no fluid
splashes on the neck of the receiving flask. It is important that the
neck of the flask and its stopper remain dry throughout the
experiment.
The pipette must be held vertically. Allow to drain for 10 s before
removing the pipette. Do not blow out the last drop.
READ page 729, Analytical Chemistry,
Gary.D Christian or other current
analytical textbook / YOUTUBE VIDEOS
45

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BURETTE

A burette is used for the accurate delivery

of a variable amount of solution
Burette enable the analyst to deliver any
volume up to their maximum capacities
Its principle use is in titration, where a
standard solution is added to the sample
solution until the end point is reached
The conventional burette for microtitration
is marked in 0.1 ml increments from 0 to
50 ml. The volume delivered can be read to
the nearest 0.05 ml by interpolation.
46

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READING BURETTE

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BASIC TECHNIQUES FOR USING BURETTE

Clean the burette with detergent and water and
rinse it with distilled water.
Check the bore and tip are clear.
Rinse twice with 5-10 mL portions of the intended
solution.
Using a funnel, fill with the intended.
Displace any air bubbles from the tip of the
burette, and adjust to near zero mark. Allow to
stand for a few minutes to check for leakage and
read the initial volume to the nearest 0.05mL.

READ page 729, Analytical

Chemistry, Gary.D Christian
or other current analytical
textbook / YOUTUBE VIDEOS

48

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VOLUMETRIC FLASK
Volumetric flasks are used in the diluting of a
sample or solution to a certain volume.
The volumetric flasks come in a variety of sizes,
ranging from 1.0 mL or more to 2.0 L.
The flask are designed to contain an accurate
volume at the specified temperature (20 or 25
C).
These flasks are marked with TC to indicate
to contain

49

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TECHNIQUES FOR USING VOLUMETRIC FLASK

Initially a small amount of diluent (usually

distilled water) is added to the empty flask.
REAGENT CHEMICALS SHOULD NEVER BE
ADDED DIRECTLY TO A DRY FLASK SURFACE,
as glass is highly absorbent to concentrated
substances.
Then the desired chemical reagent (either solid
or liquid) is added to the flask.

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Then the diluent (dilution solvent) is added to fill

flask about 2/3 and flask is swirl to mix it before
diluent is further added to the neck of the flask.
Finally diluent is added to the meniscus carefully
in dropwise manner.
The solution is finally thoroughly mix by inverting
the flask and swirl or shake vigorously for 10 sec.
Turn right side-up and repeat the invertion,
shaking or swirling for at least 10 times.

51

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STEPS IN PREPARING STANDARD SOLUTION

52

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OTHER TYPES OF GLASSWARES

53

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CALIBRATION OF GLASSWARES
.

RELATIVE
Volumetric relationship
between two items of
glassware without
knowing the absolute
volume of either. This
situation arise, for
example, in taking an
aliquot portion of a
solution.

INDIRECT

DIRECT
A volume of water
delivered by a buret
or pipet, or
contained in a
volumetric flask, is
obtained directly
from the weight of
the water and its
density

Volumetric glassware
calibrated by comparison of the
mass of water it contains or
delivers at a particular
temperature with that of
another vessel which had been
calibrated directly.
The volumes are directly
related to the masses of water.
This method is convenient if
many pieces of glassware are
to be calibrated.

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CALIBRATION OF A 50 ML VOLUMETRIC PIPETTE

Ensure the pipette is clean.

Determine the mass of the empty, stoppered receiver to
the nearest milligram.
Transfer the 50 mL volume from pipette into a stoppered
container.
Weigh the stoppered receiver and its contents and
calculate the mass of water delivered by difference.
From the delivered mass of water, calculate the volume
delivered using the appropriate density data table.
Repeat the calibration three times and calculate the
mean volume delivered and the standard deviation.

55

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CLEANING OF GLASSWARE
Clean glassware is imperative for accurate and
precise volumetric applications.
It is therefore necessary to thoroughly clean all
glassware before use.

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Warm
Detergent

Potassium
dichromate
sulphuric acid
cleaning
solution

Aqua regia
cleaning
solution (nitrohydrochloric
acid)

Method for
Cleaning
Glassware

Concentrated
Acid

Ultrasonic
cleaning

57

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

DISTILLED WATER

Distilled water is desirable as it contain no

dissolved minerals, chemicals, impurities etc.

The water distiller effectively removes more

than 99.8% of most tap water impurities,
including crystosporidium. (Cryptosporidium is a
genus of apicomplexan protozoans that can cause
gastrointestinal illness with diarrhea in humans.)

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DISTILLATION PROCESS
A.
B.
C.

D.
E.

The dirty water is heated,

To boiling thus vapourises
(becomes steam), while
other substances remain in
solid state in boiler. Steam is
then directed into a cooler,
Where it cools down and
return to liquid water,
And the end result is a
water, purified of additional
substances in it.
60

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Q
What is distilled water?
What will be removed from distillation?
What cannot be removed from distillation and
why?
What will happen to the boiler after period of time?
What will you do?
What other applications of distilled water besides
using in laboratory?

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DEIONIZED WATER
The deionization process
removes ions from water
via ion exchange.

H+
H+
H+
Na+

The vast majority of dissolved impurities

in modern water supplies are ions as
calcium, sodium, chlorides etc.

Na+, Cl-

Positively charged ions (cations) negatively

charged ions (anions) are exchanged for
hydrogen (H+) and hydroxyl (OH-) ions,
respectively, due to the resins greater affinity
for other ions.

OHOHOHCl-

H+, OHThe ion exchange process

occurs on the binding sites of
the resin beads.

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PROCESS IN DEIONIZED WATER

The vast majority of dissolved impurities in modern water
supplies are ions as calcium, sodium, chlorides etc.
The deionization process removes ions from water via ion
exchange.
Positively charged ions (cations) negatively charged ions
(anions) are exchanged for hydrogen (H+) and hydroxyl (OH-)
ions, respectively, due to the resins greater affinity for other
ions.
The ion exchange process occurs on the binding sites of the
resin beads.
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Q
What is deionized water?
What will be removed from the ion exchange
process?
What cannot be removed from ion exchange
and why?
What are the application of deionized water?

64

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

HEATING APPARATUS

Heating
apparatus

Electric
Oven

Lab Oven

Lab Bunsen
burner

Electric
furnace

Microwave
Oven

Hotplate

Memmert
drying oven

66

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TYPES OF HEATING APPARATUS

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DESICCATORS OR DESICCANT DRY CABINET

Vacuum dessicators

XDesiccant

dry cabinet

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Desiccators or desiccant dry cabinet is an

enclosure with a supply of desiccant which
maintains an internal environment of 1-20% RH
(relative humidity)
Desiccant itself is defined as: A substance that
has a high affinity for water and is used as a drying
agent .
Commercially, desiccant materials are supplied as:
Montmorillaonite clay, silica gel, molecular sieve,
calcium oxide, calcium sulfate and zeolite.

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APPLICATIONS OF DESICCATORS
Prevention and protection against all types of
oxidation (rust)
The prevention of the growth of fungus on
optics
The dry preservation of lab materials and
samples as well as the protection of MSDs
(moisture sensitive devices) in electronic
industry.

70

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

FILTRATION APPARATUS AND TECHNIQUES

Filtration is a technique used either to remove
impurities from a solution or to isolate any
solid.
The two type of filtration commonly used in
chemical labs are:

1.
2.

GRAVITY FILTRATION
VACUUM FILTRAION

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GRAVITY FILTRATION

FOLD THE PAPER INTO A CONE BY FIRST

FOLDING IT IN HALF, AND THEN IN HALF AGAIN,
AS SHOWN.

73

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FILTERING THE SOLUTION

Support the glass funnel in a ring or place it in

the neck of an Erlenmeyer flask.

74

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FLUTED FILTER PAPER

Usually used to filter hot solution.
Hot filtration helps to remove
insoluble impurities.

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VACUUM FILTRATION
Vacuum filtration is primarily used to collect a
desired solid, for instance, the collection of
crystals in a recrystallization procedure.
Vacuum filtration uses either a Buchner or a
Hirsh funnel.
It is fater than gravity filtration, because the
solvent or solution and air is forced through
the filter paper by the application of reduced
pressure.

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VACUUM FILTRATION (FILTERING BY SUCTION)

Buchner funnel + filter papeer

Other filtering devices: porcelain, glass
aluminium oxide

77

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VACUUM FILTRATION APPARATUS

78

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85

Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques

TOPIC 2
Apparatus & Techniques

ZK_CHM421

TITRATION APPARATUS AND TECHNIQUES

A titration is a method of analysis that will
allow you to determine the precise endpoint
of reaction and therefore the precise
quantity of reaction in titration flask.
Buret is used to deliver the second reactant
to the flask.
Indicator is used to detect the endpoint of
reaction.

87

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TITRATION APPARATUS AND TECHNIQUES

88

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Titrant
Analyte
Titre

89

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CHEMICAL REAGENTS

Purity of reagents has an important effect on

the accuracy of the chemical analysis
Classifying
chemicals

Reagent grade (GR)

Special-purpose
reagent chemicals
(Prepared for specific
application. E.g. spectroscopic
solvents and HPLC solvents)

Primary standard grade

(AnalaR)

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RULES FOR HANDLING REAGENTS AND

SOLUTIONS
Select the best suitable grade of chemicals
available for analytical work. Pick the smallest
bottle to supply the desired quantity (prevent
wastage and overdue)
Replace caps of the reagent bottle immediately
after use.
Hold the stopper of the reagents bottles between
your fingers; never set a stopper on the table.
NEVER RETURN ANY EXCESS REAGENTS TO A
BOTTLE.

92