Handling Chemical Reagents
Classification of Chemicals:
Reagent Grade – chemicals conform to the minimum
standards set by the Reagent Chemical Committee of
the American Chemical Society (ACS)
Primary-Standard Grade – highly purified compound
that serves as reference material
Special-Purpose Reagents – chemicals were prepared
for a specific application (i.e. solvents for
spectrophotometry or HPLC)
Requirements of Primary Standard
1. High purity (preferably 99.9% or better)
2. Stable; can withstand heating and does not react with
normal atmospheric substances
3. Absence of hydrate water
4. Modest cost
5. Reasonably soluble in the titration medium
6. Has large molar mass to minimize relative error
associated with weighing
Rules in Handling Reagents & Solutions
Pick the smallest bottle that will supply the desired
quantity.
Immediately cover the container after use.
Hold stoppers of reagents bottles between fingers.
Never return excess reagent to a bottle.
Use clean porcelain spatula for getting solid reagents.
Immediately clean up spills.
Observe proper disposal of reagents and chemical
wastes.
Cleaning of Glasswares
Rinse with: warm detergent solution, tap H2O & dH2O
Properly cleaned glassware – coated with uniform and
unbroken film of water
Drying – potential source of contamination
Measuring Mass
Weighing balance – designed to particular type of
application
Important specifications of a balance:
- Accuracy
- Precision
- Capacity – refers to the max weight that the balance can
measure
- Sensitivity – smallest weight that will produce a certain
measurable response
- Readability – smallest discernible scale division
Measuring Mass
For weighing the mass of a sample, you’ll be instructed
to:
Weigh roughly
Weigh accurately
Techniques in Weighing
Direct weighing
Taring – setting the balance to read zero in
the presence of an empty sample container.
Weighing by difference – useful for series of
sample weights; used for weighing hygroscopic
or volatile substances
TRIPLE BEAM BALANCE
Use for rough weighing
Sensitivity – 0.01g, Readability – 0.1g
Parts of a TRIPLE BEAM BALANCE
Balance Pan Riders Pointer
Adjustment Screw Scale
Analytical Balance
Capable of weighing
objects with a very
high degree of
accuracy and precision
Can give the mass of a
sample up to 0.0001 g
Limited amount of
sample may be
weighed
Parts of an Analytical Balance
Draft Shield Doors
Balance Pan Control Panel
Mass Readout
Adjustment Screw
Weighing using Analytical Balance
The bubble in the spirit level should be within the
black circle.
The object being weighed should not be touched with
bare hands.
Objects should be at room temperature before being
weighed.
Center the load on the pan as possible.
Close the sliding doors before reading the weight.
Protect the pan from corrosion.
Clean the device after using.
Spirit Level
Loading of
sample on
the analytical
balance
Control Panel of Analytical Balance
Type of Calibration of
Volumetric Equipment
TD (to deliver)
Pipets and burets
TC (to contain)
Volumetric flasks
Volumetric Flasks
The etched mark on the neck
of the volumetric flask has
been calibrated by the
manufacturer
used to measure very precisely
one specific volume of liquid
Using a Volumetric Flask:
Preparing a Flask for Use
The best way to eliminate water clinging
to the walls of the flask is to wash the
flask with laboratory soap and rinse it
thoroughly
Do not attempt to dry the flask with a
paper towel.
Rinse the flask several times with the
solvent that will be used to prepare the
solution.
Using a Volumetric Flask:
Filling a Volumetric Flask Properly
1. Transfer the solution to be diluted
to the volumetric flask, and then
fill the volumetric flask to
approximately 3/4 of its total
volume.
2. Slowly add the solvent drop-wise
with a medicine dropper. Allow
enough time between drops for
the solvent to flow down the
neck of the flask.
Using a Volumetric Flask:
Filling a Volumetric Flask Properly
3. When the solution nears the calibration mark, the
meniscus should be viewed at eye level to
eliminate parallax.
4. Continue the drop-wise addition until the bottom
of the meniscus is touching the calibration mark.
Reminders in using Volumetric Flasks
Mix the solution using the glass/plastic stopper
Mix the solution very well
Do not use as a container for long storage
Filling a Mohr Pipet
1. Use a bulb to 2. Keep the
draw liquid tip below
into the the liquid
pipet. surface.
3. Remove the 4. Touch off
bulb and the
seal the hanging
pipet with drop.
your index
finger.
Reminders in using Pipettes
Make sure the pipettes are clean before using
Use different pipettes for different solutions
Reading a Buret Properly
1. Read meniscus at eye level.
WRONG WRONG
Reading a Buret Properly
2. Use a contrast card to see the meniscus of a pale-colored or
colorless solution.
Reading a Buret Properly
3. For darker liquids, read
the bottom of the
meniscus if visible.
If not, read the top of the
meniscus.
Reporting Quantitative Data
In reporting data – include all
digits that are known with
certainty plus the first
uncertain digit.
Example:
3.70 mL
Buret Preparation
A cracked buret is inspected and rejected
Buret Preparation
A stopcock should be inspected and adjusted if necessary
Buret Preparation
A dirty buret causes contamination
Washing a Buret
The person washes the buret with a buret brush and a soap solution
Rinsing a buret
1. Rinse the buret with 5 mL
distilled water
2. Carefully, hold the buret
horizontally over a sink and
rotate the buret
3. Repeat the procedure for 3
times
4. A small amount of detergent
could be used to clean burets
that will not clean up with
distilled water
Filling a Buret
stopcock is closed
clamp the buret into place
waste beaker underneath the
buret
carefully fill the buret with the
titrant
Fill the buret to near the 0.00
mL mark, being careful to not
overfill the buret
Prepare for Titration
The final liquid level is above the
Fill the buret with titrant
top graduation mark
Prepare for Titration
remove the buret from the
stand
holds it over a waste
container
opens the stopcock and the
volume is adjusted to the
desired level
There should be no bubble
in the top of the buret tip
Bubbles on the tip
bubble in the top of the Fully open the stopcock
tip of the buret
Titration Proper
A. Control of the buret (Geissler)
Right hand controls the stopcock; left hand swirls the flask
Left hand controls the stopcock; right hand swirls the flask
*Mohr buret-different technique
B. Drop ;stop; swirls/simultaneous dropping and swirling
C. Monitor the volume used/consumed
Initial reading (IR)
Final reading (FR)
Volume consumed = FR-IR
Titrating Near the Endpoint
Take note of development of persistent color
Use half-drop method
Take note of the volume before adding more
titrant
Wash sides of the E.flask containing the
analyte solution with distilled water
