Chemical Apparatus, and Unit

Operation of Analytical Chemistry

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 spectrophotometry and
high-performance liquid chromatography.
 Rules for Handling Reagents and
Solutions

1. Select the best grade of chemical available

for analytical work.
2. Replace the top of every container
immediately after removal of the reagent.
3. Hold the stoppers of reagent bottles
between your fingers.
4. Never return any excess reagent to a bottle.
 Rules for Handling Reagents and
Solutions

5. Never insert spatulas, spoons, or knives into

a bottle that contains a solid chemicals.
6. Keep the reagent shelf and the laboratory
balance clean and neat.
7. Observe regulations concerning the disposal
of surplus reagents and solutions.
 Cleaning and Marking Laboratory Ware

• Every beaker, flask, or crucible that will contain the

sample must be thoroughly cleaned before being
used.
• The apparatus should be washed with a hot detergent
solution and then rinsed, initially with tap water and
finally with several small portions of deionized
water.
• Organic solvents such as benzene or acetone may be
used to remove grease films.
 Types of Analytical Balances

An analytical balance is a weighing

instrument with a maximum capacity that
ranges from 1 g to a few kilograms with a
precision of at least 1 part in 105 at
maximum capacity.

Macrobalances have a maximum capacity

ranging between 160 and 200 g;
measurement can be made with a standard
deviation of 0.1mg.
 Types of Analytical Balances

Semimicroanalytical balances have a

maximum load of 10 to 30 g with a precision
of 0.01mg.
Microanalytical balance has a capacity of 1
to 3 g and a precision of 0.001mg.
 Desiccators and Desiccants

• Oven drying is the most common way of

removing moisture from solids.

• This approach is not appropriate for

substances that decompose or for those from
which water is not removed at the
temperature of the oven.
 Desiccators and Desiccants

• Dried material are stored in desiccator while

they cool so as to minimize the uptake of
moisture.

• The base section of the desiccator contains a

chemical drying agent (desiccants) such as
anhydrous calcium chloride, calcium sulfate,
magnesium perchlorate or phosphorus
pentoxide.
Desiccator
 Weighing by Difference

Weighing by difference is a simple method for

determining a series of sample weights.
• First the bottle and its contents are weighed.
• 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.
• Following transfer, and its residual contents are
weighed.
• The mass of the sample is the difference
between the two weighings.
Weighing bottles
 Volume Measurement
 Pipets

 Burets

 Volumetric flask

 Measuring cylinder
Typical pipets
Automatic pipet
Burets and volumetric flask
Reading a buret
Using pipet
Titration
 Simple Crucibles

Simple crucibles serve only as containers.

Porcelain, aluminum oxide, silica and platinum
crucibles maintain constant mass and are used
principally to convert a precipitate into a suitable
weighing form.
• The solid is first collected on filter paper.
• The filter and contents are then transferred to a
weighed crucible,
• the paper is ignited.
 Filtering Crucibles

Filtering crucibles serve not only as containers but also

as filters.
• A vacuum is used to hasten the filtration
• a tight seal between crucible and filtering flask is
accomplished with any of the several types of rubber
adapters.
Filtering Crucible
 Sintered-glass Crucibles
Sintered-glass crucibles are manufactured in fine,
medium, and coarse porosities. The upper temperature
limit for sintered glass crucible is ordinarily about
200oC. Filtering crucibles made entirely of quartz can
tolerate substantially higher temperatures.

Filter Paper
Paper is an important filtering medium. Ashless paper is
manufactured from cellulose fibers that have been
treated with HCl and HF acids to remove metallic
impurities and silica, NH3 is then used to neutralize the
acids. It is necessary to destroy the paper by ignition if
the precipitate collected on it is to be weighed.
Decantation and transferring precipitate
Folding and seating a filter paper
Vacuum Filtration
 Heating Equipment

Many precipitate can be weighed directly after being

brought to constant mass in a low temperature drying
oven.

Such an oven is electrically heated and capable of

maintaining a constant temperature to within 1oC. The
maximum attainable temperature ranges from 140 to
260oC, depending on make and model, for many
precipitate 110oC is a satisfactory drying temperature.
 Heating Equipment

Microwave laboratory ovens are currently appearing

on the market. Where applicable, these greatly
shorten drying cycles.

Muffle furnace (a heavy duty electric furnace) is

capable of maintaining controlled temperatures of
1100oC or higher. Long handled tongs and heat
resistance gloves are needed for protection.
 Calibrating Glassware

Volumetric glassware is calibrated by measuring

the mass of a liquid (water) of known density
and temperature that is contained in the
volumetric ware.
 Laboratory Notebook
1. Record all data and observations
2. Supply each entry with a heading
3. Date each page of the notebook
4. Never attempt to erase an incorrect entry, cross
it out with single horizontal line
5. Never remove a page from the notebook
6. Do not overcrowd entries
7. Keep first few pages for table of contents
Lab note book