Introduction:

At the heart of analytical chemistry is a core set of operations and equipment. This set is
necessary for laboratory work in the discipline and serves as the foundation for its growth and
development. Mastery of the tools of analytical chemistry will serve well in chemistry courses and in
related scientific fields. In addition, efforts will be rewarded with the considerable satisfaction of having
completed an analysis with high standards of good analytical practice and with levels of accuracy and
precision consistent with the limitations of the technique.

Classification of chemicals
1. Reagent grade
2. Primary-standard grade
3. Special-purpose reagent chemicals

Rules for Handling Reagents and Solutions

1. Select the best grade of chemical available for analytical work. Whenever possible, pick the
smallest bottle that is sufficient to do the job.
2. Replace the top of every container immediately after removing reagent. Do not rely on someone
else to do so.
3. Hold the stoppers of reagent bottles between your fingers. Never set a stopper on a desk top.
4. Unless specifically directed otherwise, never return any excess reagent to a bottle. The money
saved by returning excesses is seldom worth the risk of contaminating the entire bottle.
5. Unless directed otherwise, never insert spatulas, spoons, or knives into a bottle that contains a
solid chemical. Instead, shake the capped bottle vigorously or tap it gently against a wooden table
to break up an encrustation. Then pour out the desired quantity. These measures are
occasionally ineffective, and in such cases a clean porcelain spoon should be used.
6. Keep the reagent shelf and the laboratory balance clean and neat. Clean up any spills
immediately.
7. Follow local regulations concerning the disposal of surplus reagents and solutions.

Marking of Laboratory Ware

1. Flasks, beakers, and some crucibles have small etched areas on which semi-permanent
markings can be made with a pencil.
2. Special marking inks are available for porcelain surfaces. The marking is baked permanently into
the glaze by heating at a high temperature. 
3. A saturated solution of iron(III) chloride, although not as satisfactory as the commercial
preparation, can also be used for marking
4. If the glassware doesn’t have an etched area, gummed label can be used and placed in the body
of the glassware.

Cleaning Laboratory Ware

1. The apparatus should be washed with a hot detergent solution and then rinsed—initially with
large amounts of tap water and finally with several small portions of deionized water.
2. Properly cleaned glassware will be coated with a uniform and unbroken film of water. It is seldom
necessary to dry the interior surface of glassware before use. Drying is usually a waste of time
and is always a potential source of contamination. (Unless you are directed otherwise, do not dry
the interior surfaces of glassware or porcelain ware).
3. An organic solvent, such as methyl ethyl ketone or acetone, may be effective in removing grease
films.

Measuring Mass
1. Equipment/Apparatus
1. Analytical Balances
1. Microbalance
 2. Semimicroanalytical balance
3. Microanalytical balance
4.Equal-arm balance
5. Single-pan analytical balance
6. Electronic analytical balance

b. Weighing bottles
1. Desiccators
2. Desiccants
2. Parts of analytical balance

3. Using analytical balance

a. Do not use aggressive cleaning agents. Clean with a mild soap, and polish with a dry
cloth.
b. Calibrate your balance at the location where it will be used. Re-calibrate on a regular
basis and any time the balance is moved
c. Operate your balance in an environment where the ambient temperature is maintained
between 180C and 300C.
d. Avoid vibrations by placing your balance on a stable surface in a draft-free location.
e. Use a leveling bubble and adjustable foot screws to ensure your balance is completely
level.
f. Place a discharge ionizer next to your balance to prevent electrostatic charge from
distorting weighing results.
g. Keep the door shut to isolate the weighing pan from the lab environment.
h. Avoid touching the sample pan with bare hands by wearing gloves.

Measuring Volume
1. Pipet
1. Volumetric
2. Mohr 
3. Serological 
4. Ostwald-Folin
5. Lambda
6. Eppendorf
a) volumetric pipet, (b) Mohr pipet, (c) serological pipet, (d) Eppendorf micropipet, (e) Ostwald–Folin
pipet, (f ) lambda pipet.

1. Directions for Using a Pipet

a. Aspirating
 Liquid is drawn into a pipet through the application of a slight vacuum. Never
pipet by mouth because there is risk of accidentally ingesting the liquid being
pipetted. 
 Instead, use a rubber suction bulb or one of a number of similar, commercially
available devices.
 A meniscus - is the curved surface of a liquid at its interface with the atmosphere.
In reading volumes, the eye must be at the level of the liquid surface to avoid an
error due to parallax. Parallax is a condition that causes the volume to appear
smaller than its actual value if the meniscus is viewed from above and larger if
the meniscus is viewed from below.

b. Dispensing an aliquot. 
 Draw a small amount of the liquid into the pipet and 
  wet the interior surface of the glass by tilting and rotating the pipet. Repeat this
procedure two more times. Then draw liquid into the pipet so that the level is a few
centimeters above the line etched on the stem of the pipet. While holding the tip of
the pipet against the inside surface of the volumetric flask,
 allow the liquid level to descend until the bottom of the meniscus is aligned with the
line (d). Remove the pipet from the volumetric flask, tilt it 
 until liquid is drawn slightly up into the pipet, and wipe the tip with a lintless tissue as
shown. Then while holding the pipet vertically, 
 allow the liquid to flow into the receiving flask until just a small amount of liquid
remains in the inside of the tip and a drop remains on the outside. Tilt the flask
slightly as shown in (g), and finally, touch the tip of the pipet to the inside of the flask.
 When this step is completed, a small amount of liquid will remain in the pipet. Do not
remove this remaining liquid. The pipet is calibrated to reproducibly deliver its rated
volume when this liquid remains in the tip.

2. Burette
a. Glass-bead valve
b. Teflon valve

2.1. Directions for Using a Burette

 a. Cleaning
b. Lubricating a Glass Stopcock
c. Filling
d. Titration

3. Volumetric Flasks
a. To contain
b. To deliver 
1. Directions for Using a Volumetric Flask
a. Direct Weighing into a Volumetric Flask
b. Quantitative Transfer of Liquid to a Volumetric Flask
c. Diluting to the Mark

General Directions for Calibration

1. Calibrating a Volumetric Pipet
a. Determine the empty mass of the stoppered receiver to the nearest milligram. 
b. Transfer a portion of temperature equilibrated water to the receiver with the pipet, weigh the
receiver and its contents (again, to the nearest milligram), and calculate the mass of water
delivered from the difference in these masses. 
c. With the aid of Table below, calculate the volume delivered. 
d. Repeat the calibration several times, and calculate the mean volume delivered and its standard
deviation.
2. Calibrating a Burette
a. Fill the burette with temperature-equilibrated water and make sure that no air bubbles are trapped
in the tip. 
b. Allow about 1 minute for drainage, and then lower the liquid level to bring the bottom of the
meniscus to the 0.00-mL mark. 
c. Touch the tip to the wall of a beaker to remove any adhering drop. 
d. Wait 10 minutes and recheck the volume. If the stopcock is tight, there should be no perceptible
change. During this interval, weigh (to the nearest milligram) a 125-mL conical flask fitted with a
rubber stopper.
e. Once tightness of the stopcock has been established, slowly transfer (at about 10 mL/min)
approximately 10 mL of water to the flask. 
f. Touch the tip to the wall of the flask. Wait 1 minute, record the volume that was apparently
delivered, and refill the burette. 
g. Weigh the flask and its contents to the nearest milligram. The difference between this mass and
the initial value is the mass of water delivered. Use
h. Using the table below convert this mass to the true volume. 
i. Subtract the apparent volume from the true volume. 
j. This difference is the correction that should be applied to the apparent volume to give the true
volume. 
k. Repeat the calibration until agreement within 60.02 mL is achieved.
l. Starting again from the zero mark, repeat the calibration, this time delivering about 20 mL to the
receiver. 
m. Test the burette at 10-mL intervals over its entire volume.
n. Prepare a plot of the correction to be applied as a function of volume delivered. 
 o. The correction associated with any interval can be determined from this plot.
3. Calibrating a Volumetric Flask
a. Weigh the clean, dry flask to the nearest milligram. 
b. Then fill to the mark with equilibrated water and reweigh. 
c. With the aid of Table below, calculate the volume contained.
4. Calibrating a Volumetric Flask Relative to a Pipet
a. The calibration of a volumetric flask relative to a pipet provides an excellent method for
partitioning a sample into aliquots. 
b. These directions are for a 50-mL pipet and a 500-mL volumetric flask. Other combinations of
volumes are equally convenient. 
c. Carefully transfer ten 50-mL aliquots from the pipet to a dry 500-mL volumetric flask. 
d. Mark the location of the meniscus with a gummed label. 
e. Cover with a label varnish to ensure permanence. 
f. Dilution to the label mark permits the same pipet to deliver precisely a one-tenth aliquot of the
solution in the flask. Note that recalibration is necessary if another pipet is used.

The Laboratory Notebook

A laboratory notebook is needed to record measurements and observations concerning an
analysis.

 a. Maintaining a Laboratory Notebook

1. Record all data and observations directly into the notebook in ink. Neatness is desirable, but you
should not achieve neatness by transcribing data from a sheet of paper to the notebook or from
one notebook to another. The risk of misplacing—or incorrectly transcribing—crucial data and
thereby ruining an experiment is unacceptable.
2. Supply each entry or series of entries with a heading or label. A series of weighing data for a set
of empty crucibles, for example, should carry the heading “empty crucible mass” (or something
similar), and the mass of each crucible should be identified by the same number or letter used to
label the crucible.
3. Date each page of the notebook as it is used.
 4. Never attempt to erase or obliterate an incorrect entry. Instead, cross it out with a single
horizontal line and locate the correct entry as nearby as possible. Do not write over incorrect
numbers. With time, it may become impossible to distinguish the correct entry from the incorrect
one.
5. Never remove a page from the notebook. Draw diagonal lines across any page that is to be
disregarded. Provide a brief rationale for disregarding the page.

Safety in the Laboratory

1. Before you begin work in any laboratory, learn the location of the nearest eye fountain,
fire blanket, shower, and fire extinguisher. Learn the proper use of each, and do not
hesitate to use this equipment if the need arises.
2. Wear eye protection at all times.
3. Most of the chemicals in a laboratory are toxic, some are very toxic, and some such as
concentrated solutions of acids and bases—are highly corrosive. Avoid contact between
these liquids and the skin.
4. NEVER perform an unauthorized experiment. Unauthorized experiments are grounds for
disqualification at many institutions.
5. Never work alone in the laboratory. Always be certain that someone is within earshot.
6. Never bring food or beverages into the laboratory. NEVER drink from laboratory
glassware. NEVER smoke in the laboratory.
7. Always use a bulb or other device to draw liquids into a pipet. NEVER pipet by mouth.
8. Wear adequate foot covering (no sandals). Confine long hair with a net. A laboratory coat
or apron will provide some protection and may be required.
9. Be extremely tentative in touching objects that have been heated because hot glass
looks exactly like cold glass.
10. Always fire-polish the ends of freshly cut-glass tubing. NEVER attempt to force glass
tubing through the hole of a stopper. Instead, make sure that both tubing and hole are
wet with soapy water. Protect your hands with several layers of towel while inserting
glass into a stopper.
11.  Use fume hoods whenever toxic or noxious gases are likely to be evolved. Be cautious in
testing for odors. Use your hand to waft vapors above containers toward your nose.
12.  Notify your instructor immediately in the event of an injury.
13.  Dispose of solutions and chemicals as instructed. It is illegal to flush solutions containing
heavy metal ions or organic liquids down the drain in most localities. Alternative
arrangements are required for the disposal of such liquids