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Handling Chemical Reagents: Reagent Grade

The document discusses guidelines for safely handling chemical reagents, including classifications of chemicals, requirements for primary standards, rules for handling reagents and solutions, techniques for cleaning glassware, weighing samples using analytical balances and volumetric equipment, and procedures for titration experiments. Proper techniques are emphasized for minimizing errors and contamination when working with chemicals and laboratory equipment.

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Bruce Devela
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85 views

Handling Chemical Reagents: Reagent Grade

The document discusses guidelines for safely handling chemical reagents, including classifications of chemicals, requirements for primary standards, rules for handling reagents and solutions, techniques for cleaning glassware, weighing samples using analytical balances and volumetric equipment, and procedures for titration experiments. Proper techniques are emphasized for minimizing errors and contamination when working with chemicals and laboratory equipment.

Uploaded by

Bruce Devela
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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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

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