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CHM421 – Analytical Chemistry

Topic 2: Apparatus & Techniques
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2.1 : Balances
Analytical balance – is an instrument for determining mass with a maximum capacity that
ranges from 1 g to several kg or a given measurement agrees with the standard value to that
measurement.

Types of analytical balance:

a) Macrobalance – is the common type of analytical balance; it has a maximum load of 160
to 200 g and a precision of 0.1 g.
b) Semi micro analytical balance – has a maximum load of 10 to 30 g and a precision of
0.01 mg.
c) Micro analytical balance – has a maximum load of 1 to 3 g and a precision of 0.001 mg.
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2.1.1 : Analytical Balances

Auxillary balance
(Top pan balance)
Single pan mechanical
analytical balance Electronic analytical
balance
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2.1.1 : Analytical Balances
Leveling screw
• Screw for adjusting the level of the balance’s base.

Pan Glass case

Door access
• Flat rigid support on which the specimen is placed.

pan
Door access
• Sliding doors that provide easy access to the inside of the
glass case.

Glass case Levelling screw

• Glass box that protects the pan from air currents and
dust that might cause a false reading of the weight.
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2.1.2 : Care & use
A weighing dish, boat or Weighing bottles are used for drying
paper is used for direct samples.
weighing of samples. Hygroscopic samples are weighed by
difference, keeping the bottle capped
except when removing the sample.
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2.1.2 : Care & use

Explain what is wrong of this

situation?

The balance should not be placed

near an open window or directly
in front of the air-condition air
vent. This will cause draft (a
current of air moving in an
upward or downward direction).
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2.1.2 : Care & use

a b

Question:
Refer to picture a, b & c. Describe the situation
and its effect to the analytical balance.

c
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2.1.2 : Care & use
Always handle the analytical balance with great care.
Never drop the analytical balance,
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2.1.2 : Care & use
General rule for weighing:

 Before using the analytical balance, it should be warmed up for at least for 15
minutes.
 Before turning on, be sure that 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 to
prevent the uptake of moisture by dried objects.
 Center the substance to be weighed on the pan.
 Weigh at room temperature.
 Never place chemicals directly on the pan, but weigh them in a vessel (weighing
bottle / dish / boat / 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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2.1.2 : Care & use
Weighing of solids
Direct weighing
* A weighing dish/bottle/boat/paper
is used.
* The dish or boat weighed empty
and then with the sample.
* Direct weighing satisfactory only if
the sample is nonhygroscopic
Weighing by difference
* Solid chemical materials are usually
weighed and dried in a weighing bottle.
* Replicate weighing's are most
conveniently carried out by weighing by
difference.
* Also if the sample hygroscopic, weighing
by difference with the bottle capped
must be employed.
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2.1.2 : Care & use

Technique of weighing by difference

o The sample in the weighing bottle is weighed, and then a portion is

removed and quantitatively transferred to a vessel.

o Then the weighing bottle and the sample are reweight, and from the
difference in weight, the weight of sample calculated.

o The next sample is transferred and the weight is repeated to get its
weight by difference, and so on.
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2.1.2 : Care & use
Weighing of liquids/solution

Direct Weighing Weighing by difference

The liquid is transferred to a o By pipetting out an aliquot from

weighing vessel (eg. a weighing the weighing bottle, the inside of
bottle) which is capped to prevent the pipet must be rinsed several
evaporation during the weighing, times after transferring.
and then weighed.
o Care should be taken not to lose
any sample from the tip of the
pipet during transferring.
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2.1.2 : Care & use
Precautions in Using an Analytical Balance

o An analytical balance is a delicate instrument that you must handle with care.
o Consult with your instructor for detailed instructions on weighing with your particular model of
balance.
o Observe the following general rules for working with an analytical balance regardless of make or
model:

1. Center the load on the pan as well as possible.

2. Protect the balance from corrosion. Objects to be placed on the pan should be limited to
nonreactive metals, nonreactive plastics, and vitreous, or glasslike, materials.
3. Observe special precautions for the weighing of liquids.
4. Consult your instructor if the balance appears to need adjustment.
5. Keep the balance and its case scrupulously clean. A camel’s-hair brush is useful for removing
spilled material or dust.
6. Always allow an object that has been heated to return to room temperature before weighing it.
7. Use tongs, finger pads, or a glassine paper strip to handle dried objects to prevent transferring
moisture to them.
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2.1.3 : Error in weighing (buoyancy)
o Weighing in the vacuum is the most accurate.

o The weighings that 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).

o Actually in most cases, a correction is not necessary because the error resulting from
buoyancy will cancel out in percent composition calculation.

o The same error will occur in the numerator (as the concentration of a standard solution or
weight of a gravimetic precipitate) and in the denominator (as the weight sample).

o 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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2.1.3 : Error in weighing (buoyancy)
o A buoyancy error will affect data if the density of the object being weighed differ significantly from
that of the standard weight.
o This error has its origin in the difference in the buoyant force exerted by the medium (air) on the
object and on the weights.
o Weight of object in air can be corrected to the weight in vacuum by:

dair dair
W1 = W2 + W2
dobj dwts

W1 = the corrected mass of the object

W2 = mass of the standard masses
dobj = density of the object
dwts = density of the masses
dair = density of the air displaced by masses and object = 0.0012 g cm3
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2.1.3 : Error in weighing (buoyancy)
Example 1: A bottle weighed 7.6500 g empty and 9.9700 g after introduction of an organic
liquid with a density of 0.92 g/cm3. The balance was equipped with stainless steel masses
(d = 8.0 g/cm3). Correct the mass of the sample for the effects of buoyancy. [Answer:
2.3227 g]
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2.2 : Volumetric glassware

GLASSWARE

Non
Volumetric Volumetric

TC
TD TC

To To
Deliver Contain
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2.2 : Volumetric glassware

GLASSWARE

TC TD
Volumetric
for preparation for transferring
of standard Volumetric
Pipette liquid between
solution flask containers

Graduated
cylinder Buret

for rapid measurement of liquid volume, for titration, accurate in

semi-accurate liquid measuring vessels dispensing aliquots of solution
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2.2 : Volumetric glassware

GLASSWARE

Non
Volumetric

Beaker TC
Flask

for transferring liquid to for containing a certain volume

another container
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2.2.1 : Units of volume

o The unit of volume is liter (L), is defined as one cubic decimeter.

o The milliliter (mL) is one one-thousandth of a liter (0.001 L) and is used

when the liter represents an inconveniently large volume unit.

o The microliter (μL) is 106 L or 103 mL.

o Basically, the amount of solute & solvent is measured in volume.

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2.2.2 : Pipettes

o The pipette is used to transfer a

particular volume of solution.

o It permit the transfer of accurately

known volumes from one container to
another.

o It is sometime used to deliver a certain

fraction or portion (aliquot) of a
solution.
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2.2.2 : Pipettes

1
Two common types of pipettes

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Volumetric or transfer pipette (bulb pipette)-(TD)

Sizes of 100 mL
Measuring or graduated pipette (clinical,
to 5 mL or less.
Mohr or serological pipet)-(TC)

The measuring pipettes

range from a total
volume of 25 to 0.1 mL.
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2.2.2 : Pipettes
Techniques for using a
pipet
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2.2.3 : Burettes
o A burette is used for the accurate delivery of a
variable amount of solution.

o Burette enable the analyst to deliver any volume

up to their maximum capacities.

o Its principle use is in titration, where a standard

solution is added to the sample solution until the
end point is reached.

o The conventional burette for macrotitration is

marked in 0.1 mL increments from 0 to 50 mL.
The volume delivered can be read to the nearest
0.01 mL by interpolation.
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2.2.3 : Pipettes
Techniques for using a
burette
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2.2.4 : Volumetric flask
o Volumetric flasks are used in the diluting of a
sample or solution to a certain volume.

o The volumetric flasks come in a variety of

sizes, ranging from 1.0 mL or more to 2.0 L.

o The flask are designed to contain an accurate

volume at the specified temperature (20 or
25oC).

o These flasks are marked with “TC” to indicate

“to contain”.
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2.2.4 : Volumetric flask

Techniques for using a volumetric flask

o Initially, a small amount of diluent (usually distilled water ) is added

to the empty flask.

o REAGENT CHEMICALS SHOULD NEVER BE ADDED DIRECTLY TO A

DRY FLASK SURFACE, as glass is highly absorbent to concentrated
substances.

o Then the desired chemical reagent (either solid or liquid) is added

to the flask.
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2.2.4 : Volumetric flask
Techniques for using a volumetric flask
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Other types of glassware
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Calibration of glassware
Volumetric relationship between two items of
glassware without knowing the absolute volume
RELATIVE of either. This situation arises, for example, in
taking an aliquot portion of a solution.

INDIRECT
o Volumetric glassware calibrated
CALIBRATION OF GLASSWARE by comparison of the mass of
water it contains or delivers at
a particular temperature with
that of another vessel which
DIRECT had been calibrated directly.

A volume of water delivered by a o The volumes are directly

buret or pipet, or contained in a related to the masses of water.
volumetric flask, is obtained directly This method is convenient if
from the weight of the water and its many pieces of glassware are to
density. be calibrated.
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Cleaning glassware
Aqua regia Concentrated acid
cleaning solution

Method for
warm detergent
Cleaning Ultrasonic
glassware cleaning

Potassium dichromate
sulphuric acid
cleaning solution
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2.3 : Water for laboratory use
Distilled water

o Distilled water is desirable as it contain no

dissolved minerals, chemicals, impurites,etc.

o The water distiller effectively removes more

than 99.8% of most tap water impurities,
including cryptosporidium.

Think!
 What can’t be removed from distillation and WHY?
 What will happen to the boiler after period of time?
 What the other applications of distilled water besides
using in laboratory?
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Distillation process
A > the dirty water is heated
B > to the boiling point and thus vaporizes
C C > (becomes steam), while other substances remain in solid state, in
boiler. Steam is then directed into a cooler .
B
D > where it cools down and returns to liquid water
E > and the end result is a water, purified of additional substances
D
found in it before distillation

E
A
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2.3 : Water for laboratory use
Deionized water

o Deionized water is a type of water which removed all of its ions, and it has no charge.

o It can be created by taking conventional water and letting it exposed to electrically charged resins that
will bind and attract to salts, and remove them from the water

o Uses:
 analytical blanks
 calibration standards
 chemistry experiments
involving ionic compounds
 solutions preparation
 Preparation of electrolytes for
alkaline and acid-based
batteries
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Deionized water process
A. The vast majority of dissolved
impurities in modern water
OH- + supplies are ions such as calcium,
H+ A OH- + sodium, chlorides, etc.
H+ Na OH- +
CI- B. the deionization process removes
H+ B + CI- B +
ions from water via ion exchange.
Na+
C. Positively charged ions (cations)
and negatively charged ions
C (anions) are exchanged for
hydrogen (H+) and hydroxyl (OH-)
ions, respectively, due to the
resin's greater affinity for other
ions.
H+ OH- D
D. The ion exchange process
occurs on the binding sites of
the resin
beads.
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2.4 : Heating apparatus

Heatingapparatus Heating
mantle
Electricoven
Hotplate
Laboratory
Electricfurnace
oven
Microwaveoven
Memmert
dryingoven LabBunsenburner
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2.4 : Heating apparatus
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2.5 : Dessicators
o Desiccators are sealable enclosures containing desiccants used
for preserving moisture-sensitive items such as cobalt chloride
paper for another use.

o A common use for desiccators is to protect chemicals or samples

which are hygroscopic or which react with water from humidity.
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2.5 : Dessicators
o Desiccators or Dessicant Dry Cabinet is an enclosure with a supply of desiccant which maintains an
internal environment of 1-50% RH (relative humidity).

o Desiccant itself is defined as: A substance that has a high affinity for water and is used as a drying
agent – from the Latin word desiccans.

o Commercially, desiccant materials are supplied as; Montmorillonite Clay, Silica Gel, Indicating
Silica Gel, Molecular Sieve, Calcium Oxide, Calcium Sulfate and Zeolite.

o Specific applications:

 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) ~ electronics industry.
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2.6 : Filtration apparatus & techniques

o Filtration is a technique used either to remove impurities

from a solution or to isolate any solid.

o The two types of filtration commonly used in laboratories

are:

1. Gravity filtration
2. Vacuum Filtration
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2.6 : Filtration apparatus & techniques

Gravity filtration Vacuum filtration

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2.6 : Filtration apparatus & techniques
Filter Paper

o Filter paper is used in qualitative analytical techniques to determine materials.

o There are different grades of qualitative filter paper according to different pore size.
o There are total 13 different grades of qualitative filter paper.
o The largest pore size is grade 4; the smallest pore size is grade 602 h; the most commonly used
grades are grade 1 to grade 4

Filter paper Pore size

grade
Grade 1 11 µm
Grade 2 8 µm
Grade 3 6 µm
Grade 4 20~25 µm
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2.6 : Filtration apparatus & techniques
Folding a filter paper

Simple

Pleated / Fluted
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2.6 : Filtration apparatus & techniques

Vacuum filtration

o Vacuum filtration is used primarily to collect a

desired solid, for instance, the collection of
crystals in a recrystallization procedure.

o Vacuum filtration uses either a Buchner or a

Hirsch funnel.

o Vacuum filtration is faster 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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2.7 : Titration apparatus & technique
o A titration is a method of analysis that will
allow you to determine the precise endpoint of
reaction and therefore the precise quantity of
reactant in titration flask.

o Burette is used to deliver the second reactant

to the flask.

o Indicator is used to detect the endpoint of

reaction
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2.8 : Reagents & purification of substance
CHEMICAL REAGENTS
o Purity of reagents has an important effect on the accuracy of the chemical analysis.

CLASSIFYING CHEMICALS
Laboratoty, Purified &
Technical Grade

Reagent Grade (GR) not pure enough to be offered for food,

drug, or medicinal use of any kind
acceptable for food, drug,
or medicinal use, purity  95% Primary Standard Grade (AR)
Analytical grade, stringent quality specifications,
purity  95 – 99% & better than GR

Special-Purpose Reagent Chemicals

Prepared for specific application
Examples- spectroscopic solvents and HPLC solvents.