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CHAPTER 2 CHM421

Placement Of Analytical Balance

Use Of The Analytical Balance

-Should have a stable support, usually


a concrete bench.
-Should not be placed near an open
window or directly in front of the aircondition air vent. This will cause draft.
-Should not be placed where there is
direct sunlight.
-The room should be air-conditioned.

-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 nomotion symbol switches on or off.
-Record the weight of the solute for
reference.

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.
Weighing Technique
A.DIRECT WEIGHING
B.WEIGHING BY DIFFERENCE
-Direct weighing means that an object
-Solid chemical materials are usually
is placed directly on a balance and the
weighed and dried in a weighing bottle.
mass read.
So weighing will be done directly using
-Usually use for weighing stable solid
the material in the weighing bottle.
(1 solid), non-hygroscopic and non-Replicate weighing are most
volatile liquids
conveniently carried out by weighing
-Zero balance. Place container on pan.
by difference.
Tare the balance. Place sample into
-Also if the sample is hygroscopic,
container. The weight registered on the weighing by difference with the bottle
balance is the weight of sample.
capped must be employed.
Weighing Of Liquids/Solution
Which is better?
1. Usually by direct weighing.
2. Transfer liquid to a weighing vessel
(eg. a weighing bottle has been
tared). Capped the bottle to prevent
evaporation during the weighing.

-Weighing by difference (substract


reading 1 & 2) eliminates systematic
error unlike direct weighing (weight
taken directly, or zeroing container)

CHAPTER 2 CHM421
Weigh.
3. If sample is hygroscopic, it is
weighed by difference. Pipette aliquot
from the weighing bottle, transfer into
container. The inside of the pipet must
be rinsed several times after
transferring.
4. Care should be taken not to lose any
sample from the tip of the pipet during
transfer.

-Systematic error = constant error.


Reading 1 + error from balance then
substract with reading 2 + error from
balance, thus zero error from balance.

Measuring Volume
Mohr Pipette TC
Bulb Pipette TD

Calibration Of A Volumetric Flask

Pipette

-Weigh a clean and dry volumetric flask


and record its weight.
-Fill the volumetric flask with distilled
water up to the mark and weigh the
flask again.
-Record the temperature of water.
-Calculate the mass of water in the
volumetric flask.
-Calculate the volume of water in the
flask based on the density of water at
the recorded temperature.
Basic Techniques For Using 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

-Clean the pipette with detergent and water.


-Rinse thoroughly, first with tap water then with Distilled water.
-Rinse with the intended solution, twice.
-Using 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

CHAPTER 2 CHM421
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
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.
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.
-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 drop wise 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.
Calibration of Glassware
Direct Calibration

Indirect Calibration

Relative Calibration

Volume of water
delivered by a burette or
pipet, or contained in a
volumetric flask, is
obtained directly from
the weight of the water
and its density.

Compare mass of water a


volumetric glassware
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.

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

CHAPTER 2 CHM421
Method of Cleaning Glassware
1. Potassium dichromate sulphuric
acid cleaning solution
2. Warm Detergent
3. Concentrated Acid
4. Ultrasonic cleaning
5. Aqua regia cleaning solution
(nitro-hydrochloric acid)
Filtration Apparatus And Techniques

Heating Apparatus
1.
2.
3.
4.
5.

Bunsen Burner
Hot Plate
Electric Oven
Microwave Oven
Electric Furnace

Filtration is a technique used either to remove impurities from a solution or to


isolate any solid.
Gravity Filtration
Vacuum Filtration
-Fold the paper into a cone by first
folding it in half, and then in half again
- Support the glass funnel in a ring or
place it in the neck of an Erlenmeyer
flask.

Distilled Water

-Used primarily to collect a desired


solid, for instance, the collection of
crystals in a recrystallization
procedure.
-Uses either a Buchner or a Hirsch
funnel.
-Faster than gravity filtration, because
the solvent or solution and air is forced
through the filter paper by the
application of reduced pressure
Deionised Water

-Used as it contains no dissolved


minerals, chemicals, impurities, etc.
-Water whose impurities as well as
electrolyte removed through distillation
-The Water Distiller effectively removes
more than 99.8% of most tap water
impurities since minerals and salt
remain in distillation apparatus.
-Also calls as steam distilled water
since is produced by boiling tap water
and recondensing the steam
-Removes most anions & cations
extremely pure water, unwanted ions
are removed & replaced by H+ & OH-Also removed dissolved gases
Distillation Process

-Better purity than lab distilled water

A. The dirty water is heated,


B. To boiling thus vaporises
C. (becomes steam), while other
substances remain in solid state in

A. The vast majority of dissolved


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

-Has become an essential ingredient in


many applications including Medical
laboratory, pharmaceutical, cosmetics,
electronics manufacturing, food
processing, plating, countless industrial
processes, and even the final rinse at
the local car wash.
-Does not contain ion such as Ca2+,
Na+, Cl-, Br- except H3O+ and OH-.
-Produced by an ion exchange process
Deionization Process

CHAPTER 2 CHM421
boiler. Steam is then directed into a
cooler,
D. Where it cools down and return to
liquid water,
E. And the end result is water, purified
of additional substances in it.

B. The deionization process removes


ions from water via ion exchange.
C. 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.
D. The ion exchange process occurs on
the binding sites of the resin beads.

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