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.

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.
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 acetone may be used to
remove grease films.
A chemical analysis is ordinarily performed in
duplicate or triplicate. Each vessel that holds a
sample must be marked so that its content can
be positively identified. Flask, beaker and some
crucibles have small etched areas on which semi
permanent mark can be made with a pencil.

Problem: Overheating
Bumping cause partial loss of the solution

Ans: Careful and apply gentle

heating
glass beads minimize bumping

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.
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.

Bouyancy error - density of the sample is

very much different from the standard
masses.
Temperature Effect Failure to allow
sufficient time for a heated object to return
to room temperature.

Top Loading 150 to 200 g

25,000 g
Triple Beam balance

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.
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.

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. 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. Following
transfer, and its residual contents are weighed.
The mass of the sample is the difference
between the two weighings.

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, and 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.

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 hydrochloric and
hydrofluoric acids to remove metallic impurities
and silica, ammonia 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.

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.
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.

Pipets

Burets

Volumetric flask

Measuring cylinder

Volumetric glassware is calibrated by

measuring the mass of a liquid (water) of
known density and temperature that is
contained in the volumetric ware.

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7.

Record all data and observations

Supply each entry with a heading
Date each page of the notebook
Never attempt to erase an incorrect entry,
cross it out with single horizontal line
Never remove a page from the notebook
Do not overcrowd entries
Keep first few pages for table of contents

Take a picture of 3 instruments present in

the laboratory, paste or print directly in the
bond paper with description or usage of the
instruments.