CHAPTER 2: CHEMICALS, APPARATUS,

AND UNIT OPERATIONS OF

ANALYTICAL CHEMISTRY

Main objective: We shall introduce the tools,

techniques, and chemicals that are used by analytical
chemists.
 The National Institute of
Standards and Technology
- to promote U.S. innovation
and industrial competitiveness by
advancing measurement science,
standards, and technology in ways
that enhance economic security and
improve our quality of life.
- has active programs for
encouraging and assisting industry
and science to develop and use
these standards.
Classifying Chemicals
A. Reagent Grade
- chemicals that are around 96-98% pure normally
(maximum impurity set by ACS). It’s fine for most synthesis
applications but not for pharmaceutical applications or anything
that requires very pure chemicals.
B. Primary-Standard Grade
- used in titration to determine an unknown
concentration and in other analytical
chemistry techniques.
A good primary standard meets the following criteria:
 high level of purity
 low reactivity (high stability)
 not likely to absorb moisture from the air (hygroscopic)
to reduce changes in mass in humid versus dry
environments
 non-toxic
 inexpensive and readily available
Example:
 A 1-gram sample of NaOH may not
actually contain 1 gram of NaOH
because additional water and carbon
dioxide may have diluted the solution.
 To check the concentration of NaOH, a
chemist must titrate a primary standard
(in this case a solution of potassium
hydrogen phthalate (KHP). KHP
does not absorb water or carbon
dioxide, and it can provide visual
confirmation that a 1 gram solution of
NaOH really contains 1 gram.
C. Secondary Standard Grade
 A secondary standard is a chemical that has been
standardized against a primary standard for use in a
specific analysis. NaOH, once its concentration has been
validated through the use of a primary standard, is often
used as a secondary standard.
 anything whose concentration changes with
time.
D. Special-Purpose Reagent Chemicals
- Solvents for spectrophotometry and high-performance
liquid chromatography.
Rules for Handling Reagents and Solutions
1. The best grade, the smallest bottle
2. Replace the top of every container immediately after
removal of the reagent.
3. Hold the stoppers of reagent hollies between your
fingers.
4. Never return any excess reagent to a bottle.
5. Never insert spatulas, spoons, or knives into a bottle.
6. Keep the reagent shelf and the laboratory balance clean
and neat.
7. Observe local regulations (the disposal of surplus
reagents and solution).
Cleaning and Marking Laboratory Ware
 Each vessel that holds a sample must be marked. Special marking
inks are available for porcelain surfaces. A saturated solution of
iron(III) chloride can also be used for marking.
 Every apparatus must be thoroughly 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.
 Properly cleaned glassware will be coated with a uniform and
unbroken film of water. Do not dry the interior surfaces of
glassware.
 An organic solvent, such as methyl ethyl ketone or acetone, may
be effective in removing grease films.
Evaporating Liquids
Bumping: sudden, often violent boiling that
tends to spatter solution out of its container.
Wet-ashing: Oxidation of the organic
constituents of a sample with oxidizing
reagents such as nitric acid and sulfuric
acid.The conversion of an organic compound
into ash.
Wet Ashing is treatment of the sample
with a moderate amount of sulfuric acid
before charring. Charring is performed
using an open flame. Liquid samples tend
to foam. After the excess sulfuric acid is
driven off, the sample is muffled as
above.
Measuring Mass

Analytical Balance Electronic Analytical Balance

Sources of Error in Weighing
Correction for Buoyancy
buoyancy error - weighing error that develops when the object being
weighed has a significantly different density than the weights.
W1 = W2 + W2 [(dair/dobject) –(dair/dweights)]
Ex.
 A bottle weighed 7.6500 g empty and 9.9700 g after
introduction of an organic liquid with a density of 0.92 g-cm-3. The
balance was equipped with stainless steel weights (d = 8.0 g-cm-3).
Correct the mass of the sample for the effects of buoyancy.
(dair: the density of the air displaced by them; 0.0012 g-cm-3)
mass of the liquid = 9.9700 - 7.6500 = 2.3200 g
 Temperature Effects

1. a buoyant effect on the pan and object

2. warm air trapped in a closed container weighs less than the same
volume at a lower temperature.

 Both effects cause the apparent mass of the object to be low.

 Allow heated objects to return to room temperature before being
weighed.
 Desiccators and Desiccants
 Desiccators are sealable enclosures
containing desiccants used for preserving
moisture-sensitive items such as cobalt
chloride paper for another use. A common use
for desiccators is to protect chemicals which
are hygroscopic or which react with water
from humidity.
 Desiccant: chemical drying agent, such as
anhydrous calcium chloride, calcium sulfate
(Drierile®), anhydrous magnesium
perchlorate (Anhydrone® or Dehydrite®), or
phosphorus pentoxide.
 Quantitative transfer of solid
sample. Note the use of tongs to
hold the weighing bottle and a
paper strip to hold the cap to
avoid contact between glass and
skin
 Filtration and Ignition of Solids
Apparatus
A. Simple Crucibles
- Porcelain, aluminum oxide, silica, and platinum (constant mass)
- used to heat chemical compounds to very high temperatures

B. Filtering Crucibles - containers + filters

1. Sintered-glass (fritted glass) crucibles:
porous glass through which gas or liquid may pass. It is made
by sintering together glass particles into a solid but porous body.
 The steps in filtering analytical precipitate are decantation,
washing and transferring.
C. Filter Paper
- semi-permeable paper barrier placed perpendicular to a
liquid or air flow. It is used to separate fine substances from
liquids or air. It is used in science labs to remove solids from
liquids.
D. Heating Equipment
Directions for Filtering and Igniting
Precipitates

 Preparation of a Filter
Paper
 Transferring Paper and
Precipitate to a Crucible
 Ashing Filter Paper &
Using Filtering
Crucibles
Measuring Volume
 Units of Volume
liter (L), milliliter (mL)

The Effect of Temperature on Volume Measurements

The coefficient of expansion: ≈ 0.025%/°C, standard temp: 20°C
Ex. A 40.00-mL sample is taken from an aqueous solution
at 5°C. What volume does it occupy at 20°C?
V20°C=V5°C + (0.025%/100%)(20 -5)(40.00)= 40.00+0.15=
40.15mL
Apparatus for Precisely Measuring Volume
 pipets, buret, and
volumetric flask

Pipets
A.Volumetric or transfer,
pipet - delivers a single,
fixed volume between 0.5
and 200 mL
B. Measuring pipets -
maximum capacity
ranging from 0.1 to 25
mL.
 Burets - like measuring
pipets, enable the analyst to
deliver any volume

 Volumetric Flasks: 5 mL
to 5 L
1. preparation of standard
solutions
2. dilution of samples to a
fixed volume
Using Volumetric Equipment

Cleaning
 soaking in a warm detergent solution,
tap water, distilled water. It is seldom
necessary to dry volumetric ware.

 Avoiding Parallax- This is one of the

most common errors in measurement.
Parallax error mainly happens when the
object is viewed from an angle due to
the wrong positioning of eye.
The first way to curb this error is to
orient your eyes in a straight line.Your
eyes should be in a straight line directly
above the marking on your device
Directions for Using a Pipet
 Never use your mouth to draw liquid into a pipet because of
the possibility of accidentally ingesting the liquid being
pipetted.
 Measuring an Aliquot
 The small volume remaining inside the tip of a volumetric pipet
should not be blown or rinsed into the receiving vessel.
 Directions for Using a Buret
1. Cleaning
2. Lubrication of a Glass Stopcock
3. Filling
4. Titration
Buret readings should be estimated
to the nearest 0.01 mL.

Drug titration is the process of

adjusting the dose of
a medication for the maximum
benefit without adverse effects.