SUMMER CLASS 2022-2023

ANALYTICAL CHEMISTRY

LESSON 7: FUNCTIONS OF COMMON LABORATORY ERLENMEYER FLASKS (CONICAL FLASKS)

EQUIPMENT
• Also known as a conical flask.
SAFETY GOGGLES AND SAFETY EQUIPMENT
• It has a narrow neck and expands toward its
• Safety goggles are required wear in all base.
chemistry labs.
• This allows easy mixing and swirling
• Not wearing can cause eye irritation (mechanical shaking) of the flask without too
and possibly blindness. much risk of spilling.

• A small droplet of acid could splash • The narrow opening also allows for the use of
out of the container at any time. a rubber or glass stopper.
Better safe than permanently blinded!
• IMPORTANT SAFETY TIP: never heat flask
• Latex gloves should be used all the time while it is capped, it might cause a pressure
especially when expose to corrosive build-up that could result in explosion.
chemicals.
FLORENCE FLASKS (BOILING FLASKS)
• A lab gown also prevent injury in case of spills
• Also known as a boiling flask
or splashes.
• It has a round bottom and a long neck.
• Never wear open-toed shoes or sandals in a
lab. • It is used to hold liquids and can be easily
swirled and heated.
BEAKER
• It can also easily be capped by rubber or glass
• It is used for mixing, stirring, and heating
stoppers.
chemicals.
• IMPORTANT SAFETY TIP: never heat flask
• Most beakers have spouts on their rims to aid
while it is capped, it might cause a pressure
in pouring.
build-up that could result in explosion.
• They are not a precise way to measure liquids.
VOLUMETRIC FLASKS
• Beakers come in a wide range of sizes.
• A volumetric flask is a round flask with a long
• Watch glass can be used to cover the opening neck and flat bottom.
to prevent contamination or splashing.
• It is used to measure an exact volume of
REAGENT BOTTLE liquid.

• It sometimes also referred to as media • There is a small line on the neck that indicates
bottles, are specially designed containers or how far to fill the bottle.
vessels to hold chemicals in liquid or powder
• They come with special caps that will not let
form.
anything in or out.
• They come in a variety of sizes, shapes, and
TEST TUBES
are commonly constructed of glass or plastic.
• A test tube is a glass tube with one end open
• While most are clear glass vessels, some
and the other end closed (rounded).
reagent bottles are colored amber (actinic),
brown, or red to protect light-sensitive • It used to hold small samples.
chemical compounds from visible light,
ultraviolet, and infrared radiation. • They are primarily used for qualitative
assessment and comparison.

• A common place to see these is the chemistry

lab.
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• They are generally held in a test tube rack DROPPERS

specific.
• These are small glass tubes with narrow tips
• Test-tube tongs can be used to move test on one end and a rubber bulb on the other.
tubes when it is heated.
• They suck up liquid that can then be squeezed
TEST TUBE RACKS out in small drops.

• It is use to hold test tubes while heating them. • These can be uzsed to add an indicator to a
solution about to be titrated.
• It provides a safe distance between the
person’s hand and the test tube PIPETTES

• holds the test tuXbes in an upright position. • There are a large variety of pipettes designed
to accomplish specific goals.
GRADUATED CYLINDER
• However, they are all for measuring an exact
• This is a primary measuring tool for the
volume of liquid and placing it into another
volume of a liquid.
container.
• There are several markings up and down the
length of the container with specific
increments.

• Graduated cylinders come in many sizes. The

smaller they are in diameter, the more
specific the volume measurements will be.

WATCH GLASSES

• A watch glass is just a round piece of glass

that is slightly concave/convex (think of a
lens).

• It can hold a small amount of liquid or solid.

• They can be used for evaporation purposes

and also can function as a lid for a beaker.

CRUCIBLE

• A crucible is a small clay cup made of a

material that can withstand extreme
temperatures.

• They are used for heating substances and

come with lids. BURETTE

FUNNELS • It is a glass tube that is open at the top and

• A lab funnel is just like any other funnel.
• They can be made of plastic or glass and can
have either a short stem or a long stem.
• There are several sizes that can be chosen
from based on the amount of liquid that
needs to go through them quickly.
comes to a narrow pointed opening at the
bottom.
• Right above the bottom opening is a stopcock
that can be turned to control the amount of
liquid being released.
• The markings along the length of the tube
that indicate the volume of liquid.
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ANALYTICAL CHEMISTRY
• Burettes are one of the most accurate tools in
the lab.
• Burettes are set up by using a burette clamp
in combination with a ring stand
RING STANDS, RINGS AND CLAMPS
• It is used to suspend burettes, beakers, flasks,
crucibles, etc. above other containers or in a
heat source (Bunsen burner).
• When clamping glass, be careful not to
shatter the glass.
• When using a ring on the stand, there are
other pieces necessary to accomplish the goal.
• Wire mesh - laid across the ring to
distribute evenly heat and support the
beaker.
• Clay triangle - is used to suspend
crucibles.
• Make sure everything is balanced! Do not let
the whole setup tip over.
TONGS AND FORCEPS
• Tongs and forceps are for grabbing things that
should not be touched by hand.
• Some tongs are specially made to hold
beakers, others to hold test tubes, and so on.
• There are also general tongs.
• Forceps are used to grab small things like solid
chemicals that are broken into chunks, so they
can be safely handled and added to
containers.
SPATULA AND SCOOPULAS
• It Spatulas and scoopulas are for scooping
solid chemicals.
• They are typically used to scoop a chemical
out of its original container onto a weigh boat
so that it can be weighed on a balance.
THERMOMETER
• A laboratory thermometer is used for
measuring the temperature of liquids.
• It can be made of glass or it can be a
thermocouple made of different metals.
STIRRING ROD
• Laboratory stirring rods are a piece of
laboratory equipment used to mix chemicals
and liquids.
• Stirring rods are usually made of solid or
hollow glass materials.
MAGNETIC STIRRER
• A magnetic stirrer is a device that stirs
chemical solutions by using electromagnetic
force.
• A magnetic stirring bar is inserted into the
flask containing the solution, which is then
placed over a magnetic stirrer’s hot plate.
• This method of stirring is more efficient, rapid,
and sanitary than traditional stirring with a
glass rod.
FILTER PAPER
• A filter paper is a semi-permeable sheet of
paper used in chemistry labs to separate solid
impurities or components from a liquid
solution.
• They are often made of cellulose whose
capillary function comes in handy while
separating fine solid impurities.
WASH BOTTLE
• The wash bottle is a regular plastic bottle
attached to a nozzle with a screw-top lid, and
it is used to rinse various pieces of laboratory
glassware, such as test tubes and round
bottom flasks, after or before their use.
MORTAR AND PESTLE
• Mortar and pestle are ancient tools used to
crush and grind ingredients or substances into
a thin paste or powder.
• They are used in chemistry labs to grind
chemical crystals or tablets into powder or
paste form.
BUNSEN BURNERS
• A Bunsen burner is a mechanical apparatus
that is connected to a flammable gas source.
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ANALYTICAL CHEMISTRY
• There is a knob to adjust the amount of gas
flow and a rotating collar that controls
airflow.
• These both must be adjusted to get an ideal
flame for heating purposes. The burner is lit
with a striker.
• Utmost safety is required when using a
Bunsen burner.
THE BUNSEN BURNER:
How to light the burner
Prior to Lighting Bunsen Burner:
• Know the location of the laboratory’s
main gas shut off valve and fire
extinguisher.
• Place the Bunsen burner away from
any overhead shelving, equipment, or
light fixtures by at least 12 inches.
• Remove all papers, notebooks,
combustible materials, and excess
chemicals from the area.
• Tie-back any long hair, dangling
jewelry, or loose clothing.
• Use correct tubing (butyl rubber
hose). Inspect hose for cracks, holes,
pinch points, or any defect and
replace if necessary. Ensure that the
hose fits securely on the gas valve and
the burner.
• Notify others in the lab that the
burner will be in use.
Lighting Bunsen Burner:
• Before turning on gas, have a
sparker/lighter with extended nozzle
to ignite burner. Never use matches.
• Check connections to burner and desk
outlet valve.
• Close needle valve and collar.
• Open gas valve fully.
• Open needle valve 1/2 turn.
• Use the spark/lighter to light the
flame.
• Adjust flame by turning the collar to
regulate air flow
• and produce an appropriate flame for
the experiment (typically a medium
blue flame).
During Use:
• Never leave a lighted burner
unattended. Drafts (including those
created by a hood) may extinguish the
flame, but the gas will still be on. This
could result in an explosion.
• Never face the vessel (test tube,
beaker, etc.) being used to heat a
material toward yourself or others
near the burner. In some
experiments, a hot plate may be used
in place of the Bunsen burner.
• A hot plate or heating mantle must be
used when flammable liquids are to
be heated.
After Use:
• Anything that has been heated with a
Bunsen burner is likely to be very hot.
Do not touch apparatus with your
bare hands unless the air near it feels
cool.
• If you must handle hot apparatus, use
crucible tongs or thermal gloves. Do
not set hot apparatus on paper, you
might set it on fire. Let the apparatus
cool in place, with the burner
removed or extinguished.
• Shut off gas when its use is complete.
• Allow the burner to cool before
handling. Ensure that the main gas
valve is off before leaving the
laboratory.
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TYPES OF FLAME:
Yellow Flame
• A yellow flame is also known as a
safety flame because it is easy to see
in a bright room.
• A safe flame can be achieved by fully
closing the air hole and reaches
temperature of around 300 degrees.
Blue Flame
• This flame on a burner can get as hot
as 500 degrees.
• It can be difficult to see in a bright
room ad is created when the air hole
is partially open.
Roaring Blue Flame
• The hottest setting for Bunsen flames
is the roaring blue flame.
• This is what happens when the air
hole is fully open, and can reach
temperature of 700 degrees.
BALANCES
• A balance is used to weigh chemicals.
• The chemicals are always in some form of
container and never placed directly on the
balance.
• It is important not to move a balance because
they have been calibrated for the exact
position they are in.
• Some balances have plastic housing with small
doors to keep air currents from affecting the
measurement.
• Close these doors whenever the balance is in
use.
WAYS TO MEASURE MASS
1. TRIPLE BEAM BALANCE
• The triple beam balance is an instrument
used to measure mass very precisely.
• Typically have a reading error of ±0.05 grams.
• Its name refers to its three beams, where the
middle beam is the largest, the far beam of
medium size, and the front beam the
smallest.
How to Use a Triple Beam Balance
1. Move the largest counterweight one notch at
a time until the pointer drops below zero.
2. Move the counterweight back one notch.
3. Repeat this process with the next largest
counterweight, and finally the smallest
counterweight.
4. After adjusting all three counterweights, the
pointer should be resting at zero on the scale.
Reading the balance to find the mass:
• The largest counterweight tells you the mass
to the nearest one hundred grams.
• At his balance, the largest
counterweight is on 0g, so the object
must have a mass that is less than 100
g.
• The next largest counterweight measures the
mass to the nearest ten grams.
• This counterweight is located at 40 g.
• Finally, the smallest counterweight measures
the mass to the nearest 0.1 g.
• the smallest counterweight is located
at exactly 1.0 g.
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2. ELECTRONIC BALANCE

• Electronic balance is an instrument used in

the accurate measurement of weight of
materials.

• Electronic balance is a significant instrument

for the laboratories for precise measurement
of chemicals which are used in various
experiments.

• Laboratory electronic balance provides digital

result of measurement.

How to use electronic balance Weighing by Difference

1. Place the electronic balance on a flat, stable • weighing by difference is a simple method for
surface indoors. determining a series of sample weights.

• The precision of the balance relies on
minute factors and wind, shaky
surfaces, or similar forces will cause
the readings to be inaccurate.
2. Press the "ON" button and wait for the
balance to show zeroes on the digital screen.
• first the bottle and its contents are weighed.
• one sample is then transferred from the
bottle to a container; gentle tapping of the
bottle with its top and slight rotation of the
bottle control over the amount of sample
removed.

3. Use tongs or gloves to place the empty
container you will use for the substance to be
measured on the balance platform.
• Fingerprints and other greases from
your hands add mass and must be
avoided for accurate measurements.
4. Press the "Tare" or "Zero" button to
automatically deduct the weight of the
container from future calculations. The digital
display will show zero again, indicating that
the container's mass is stored in the balance's
memory.
5. Carefully add the substance to the container.
• This is done with the container still on
the platform, but it may be removed if
necessary. Avoid placing the container
on surfaces that may have substances
which will add mass to the container
such as powders or grease.
6. Place the container with the substance back
on the balance platform if necessary and
record the mass as indicated by the digital
display.
• following transfer, and its residual contents
are weighed.
• the mass of the sample is the difference
between the two weighing.
SELECTING AND HANDLING REAGENTS AND OTHER
CHEMICALS
Classifying Chemicals
1. Reagent Grade:
Reagent grade chemical conform to the minimum
standards set forth by the Reagent Chemical
committee of the American Chemical Society and are
used wherever possible in analytical work.
2. Primary Standard Grade:
Extraordinary purity is required for a primary
standard. Primary standard reagent is carefully
analyzed and the assay is printed on the container
label.
3. Special-Purpose Reagent:
chemicals that have been prepared for a specific
application. Included among these are solvents for
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spectrophotometry and high-performance liquid (4) computation of the amount of the

chromatography. particular constituent in the sample
from the observed weight of the
RULES FOR HANDLING REAGENTS AND SOLUTIONS
isolated substance.
1. Select the best grade of chemical available
Two major types of gravimetric methods:
for analytical work.
1. Precipitation method
2. Replace the top of every container
immediately after removal of the reagent. - The analyte is converted to a sparingly soluble
precipitate.
3. Hold the stoppers of reagent bottles
between your fingers. - The precipitate is then filtered , washed free
of impurities , and converted to a product of
4. Never return any excess reagent to a bottle.
known composition by suitable heat
5. Never insert spatulas, spoons, or knives into treatment , and the product is weighed.
a bottle that contains a solid chemicals.
2. Volatilization method
6. Keep the reagent shelf and the laboratory
- The analyte or its decomposition products are
balance clean and neat.
volatilized at a suitable temperature.
7. Observe regulations concerning the
- The volatile liquid is then collected and
disposal of surplus reagents and solutions.
weighed or the mass of the product is
indirectly determined from the loss in mass of
the sample.
Cleaning and marking laboratory ware

• Every beaker, flask, or crucible that will

contain the sample must be thoroughly Gravimetric methods of analysis are based on mass
cleaned before being used. measurements with an analytical balance , an
instrument that yields highly accurate and precise
• The apparatus should be washed with a hot data.
detergent solution and then rinsed, initially
with tap water and finally with several small
portions of deionized water.
Properties of Precipitates and Precipitating Reagents
• Organic solvents such as benzene or acetone
1. readily filtered and washed free of
may be used to remove grease films.
contaminants

2. sufficiently low solubility so that no significant

LESSON 8: GRAVIMETRIC METHODS OF ANALYSIS loss of the solid occurs during filtration and
washing
Gravimetric Methods of Analysis
3. 3. unreactive with constituents of the
- are quantitative methods based on atmosphere
determining the mass of a pure compound to
which the analyte is chemically related. 4. 4. known composition after it is dried or, if
necessary ignited
The steps commonly followed in gravimetric analysis
are :

(1) preparation of a solution containing a Particle Size and Filterability of Precipitates

known weight of the sample
(2) separation of the desired constituent
(3) weighing the isolated constituent
-Precipitates made up of large particles are generally
desirable in gravimetric work because large particles
are easy to filter and wash free of impurities.
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ANALYTICAL CHEMISTRY

-In addition, such precipitates are usually purer than : When Q-S/S is small, a crystalline solid is more likely
are precipitates made of fine particles.
Supersaturated – unstable solution that contains
What Factors Determine Particle Size? more solute than a saturated solution.

1.Colloidal suspensions – tiny particles are invisible to How do Precipitate Forms?

the naked eye (10-7 to 10-4 cm in diameter.)
The effect of supersaturation on particle size can be
- the particles show no tendency to settle from explained if we assume that precipitates formed in
solution, nor are they easily filtered. two ways:

2. Crystalline suspension – temporary dispersion of 1. Nucleation

particles in the liquid phase.
2. Particle growth
- -the particles tend to settle spontaneously
and are readily filtered.
1. Nucleation
- process in which a minimum number of
atoms, ions or molecules join together to
produce a stable solid.
- a few ions, atoms, or molecules come
together to form a stable solid.
- Further precipitation involves a competition
between additional nucleation and growth on
existing nuclei (particle growth).
- Precipitates form by nucleation and particle
growth.
- If nucleation predominates, a large number of
very fine particles is produced.
- If particle growth predominates, a smaller
number of larger particles is obtained.
The particle size of a precipitate is influenced by
experimental variables: Controlling Particle Size:

1. Precipitate solubility 1. Elevated temperatures to increase the

solubility of the precipitate (S).
2. Temperature
2. Dilute solutions ( to minimize Q).
3. Reactant concentrations
3. Slow addition of the precipitating agent with
4. Rate at which reactants mixed good stirring.
Von Weiman Equation ✓ Larger particles can also be obtained by pH
𝑸−𝑺 control, provided the solubility of the
Relative supersaturation =
𝑺 precipitate depends on pH.
Q – concentration of the solute ✓ Precipitates that have very low solubilities,
S – equilibrium solubility such as many sulfides and hydrous oxides,
generally form as colloids.
Experimental evidence indicates that the particle size
of a precipitate varies inversely with the average
relative supersaturation during the time the reagent is
being introduced.

: When Q-S/S is large, the precipitate tends to be

Colloidal Precipitates
colloidal
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ANALYTICAL CHEMISTRY

- are so small that they are not retained by

ordinary filters.

- Brownian motion prevents their settling out

of solution under the influence of gravity.

Coagulation of Colloids

- can be hastened by heating, stirring, and

adding an electrolyte to the medium.

- Colloidal suspensions are stable because all particles

present are either positively or negatively charged.
This charge results from cations or anions that are
bound on the surface of the particles.
Peptization of Colloids
Adsorption – process in which a substance (gas,
liquid, or solid) is held on the surface of a solid. - a process by which a coagulated colloid
returns to its dispersed state.
✓ The adsorption of ions on an ionic solid
originates from the normal bonding forces -When a coagulated colloid is washed, some of the
that are responsible for crystal growth. electrolytes responsible for its coagulation is leached
from the internal liquid in contact with the solid
particles.

Practical Treatment of Colloidal Precipitates

➢ Digestion is a process in which a precipitate is

heated in the solution from which it was
formed (the mother liquor) and allowed to
stand in contact with the solution.

➢ Mother liquor – solution from which a

precipitate was formed.
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Crystalline Precipitates
❖ Crystalline precipitates are generally more
easily filtered and purified than are
coagulated colloids .
Methods of Improving the Particle Size and
Filterability
✓ Particle size of crystalline solids can often be
improved by significantly minimizing Q (by
using dilute solutions) or maximizing S (
precipitating from hot solution, or by
adjusting the pH), or both.
✓ Digestion improves the purity and filterability
of both colloidal and crystalline precipitates.
Coprecipitation
▪ is a process in which normally soluble
compounds are carried out of solution by
precipitate.
Four types:
➢ Surface adsorption
➢ Mixed crystal formation
➢ Occlusion
➢ Mechanical entrapment
Surface adsorption
✓ Adsorption is often the major source of
contamination in coagulated colloids but of no
significance in crystalline precipitates.
✓ In adsorption, a normally soluble compound is
carried out of solution on the surface of a
coagulated colloid. This compound consists of
the primarily adsorbed ion and an ion of
opposite from the counter-ion layer.
Reprecipitation
- In this process, the filtered solid is redissolved
and reprecipitated.
- The first precipitate usually carries down only
a fraction of the contaminant present in the
original solvent.
Mixed-crystal formation
✓ a type of coprecipitation in which a
contaminant ion replaces an ion in the lattice
of a crystal.
✓ The extent of mixed-crystal formation is
governed by the Law of Mass Action and
increases as the ratio of contaminant to
analyte concentration increases.
Occlusion
✓ type of coprecipitation in which
coprecipitated physically trap contaminated
counter ions within a precipitate during rapid
precipitate formation.
Mechanical entrapment
✓ type of coprecipitation in which
coprecipitated physically trap a pocket of
solution within a precipitate during rapid
precipitate formation
Precipitation from Homogeneous Solution
✓ Homogeneous Precipitation- a process in
which a precipitate is formed by slow
generation of a precipitating reagent
homogeneously throughout a solution.
✓ Solids formed by homogeneous precipitation
are generally purer and more easily filtered
than precipitates generated by direct addition
of a reagent to the analyte solution.
Drying and Ignition of Precipitates
➢ A gravimetric precipitate is heated is heated
until its mass becomes constant.
GRAVIMETRIC ANALYSIS REQUIREMENT
The step required in gravimetric analysis can be
summarize as follows:
i. Preparation of the solution
ii. Precipitation
iii. Digestion
iv. Filtration
v. Washing
vi. Drying or igniting
vii. Weighing
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viii. Calculation