GUIDELINES FOR LABORATORY SAFETY

All instructors, students and technicians who work in the laboratory are duty bound to
prevent exposure of themselves and others to unreasonable risks. The primary causes
of accidents in the laboratory are careless techniques, unawareness of potential
danger, improper procedures, sloppy work habits and lack of sufficient concern
for others.

Laboratory experiments can be performed with a minimum of accidents by following

established procedures.

EYE PROTECTION must be worn at ALL TIMES in areas where chemicals are
being used or stored. Safety glasses should have shatterproof lenses with splash
shields. Contact lenses are generally not safe since they can absorb chemicals that
irritate the eye. If chemicals get in your eyes flood them immediately with water and
then seek medical attention.

KNOW WHAT TO DO IN THE CASE OF AN ACCIDENT. Acquaint yourself

with the LOCATION and PROPER USE of emergency equipment such as first-aid kit,
fire extinguishers, fire blankets, safety showers and eyewash stations.

READ CAREFULLY THE EXPERIMENTAL PROCEDURE PRIOR TO

CLASS
Make note of safety warnings and precautions to be taken, equipment and techniques
to be used and the nature of the chemical substances i.e. whether they are corrosive,
volatile or poisonous. In the event of a spill apply proper procedure for cleanup and
disposal. Carefully follow the recommended manner of waste disposal of chemical
reagents and products.

USE THE FUMEHOOD WHEN HANDLING VOLATILE CHEMICALS WITH

TOXIC AND/OR IRRITATING FUMES OR WHEN CONDUCTING
EXPERIMENTS INVOLVING SUCH VOLATILE FUMES.

REPORT ALL ACCIDENTS IMMEDIATELY TO THE LECTURER IN CHARGE

OR ALERT THE NEAREST PERSON IN CASE OF AN EMERGENCY.

NEVER WORK ALONE IN THE LABORATORY OR WITHOUT IMMEDIATE

ACCESS TO ANOTHER PERSON.

KEEP YOUR WORK SPACE ORDERLY AND UNCLUTTERED.

WASH YOUR HANDS FREQUENTLY DURING AND AT THE END OF THE

LABORATORY SESSION. Fumes and chemicals may produce skin irritations after
long exposure.

1
READ LABEL OF CHEMICAL AT LEAST THREE TIMES: when OBTAINING
chemical, when MEASURING and when RETURNING to its place of origin.

ALWAYS REMEMBER TO REPLACE STOPPER OR LID OF CHEMICAL

CONTAINER AFTER USE AND TO WIPE OUTSIDE OF CONTAINER AND
WORK AREA IF ANY SPILLS HAVE OCCURRED.

NO FLAMES SHOULD BE USED DURING SESSIONS INVOLVING THE

USE OF FLAMMABLE MATERIALS, ESPECIALLY THOSE WITH LOW
BOILING POINTS.

NEVER POINT THE OPEN END OF TEST TUBES WITH REACTION

MIXTURES AT ANYONE, INCLUDING YOURSELF.

NEVER ADD WATER TO CONCENTRATED ACID. THE ACID SHOULD

ALWAYS BE ADDED SLOWLY TO THE WATER WHILE MIXING, SO
THAT ANY HEAT GENERATED CAN BE ABSORBED AND DISSIPATED.

ALWAYS BE PROPERLY ATTIRED; USE LABORATORY COATS,

COMFORTABLE WHOLE SHOES (TOES AND INSTEP COVERED) AND
KEEP HAIR TIED BACK. USE DISPOSABLE GLOVES WHEN ADVISED TO
DO SO.

DO NOT EAT, DRINK OR SMOKE IN THE LABORATORY.

REGARD EVERY CHEMICAL AS POTENTIALLY HAZARDOUS AND

VIGOROUSLY FOLLOW EVERY SAFETY PROCEDURE DESCRIBED;
THEY ARE NOT SUGGESTIONS, THEY ARE MANDATORY.

BE IN ATTENDANCE FOR LABORATORY INSTRUCTIONS AT THE

BEGINNING OF EACH SESSION AND NOTE SPECIAL PRECAUTIONS TO
BE TAKEN AND/OR CHANGES TO THE PROCEDURE, IF ANY.

ACCIDENTS ARE USUALLY PREVENTABLE. BE ALERT IN THE LAB.

Understand experimental procedures and be aware of any hazards. ASK YOUR
INSTRUCTOR TO EXPLAIN OPERATIONS YOU DO NOT UNDERSTAND.
DO NOT PROCEED UNTIL YOU KNOW WHAT YOU NEED TO DO.

BEFORE LEAVING THE LABORATORY ENSURE THAT ALL

EQUIPMENT AND ALL UTILITIES ARE TURNED OFF AND THAT YOUR
WORK AREA IS TIDY.

2
 IN CASE OF ACCIDENT

Always call or notify the laboratory supervisor as soon as possible.

Fire

1. Burning Reagents: Immediately extinguish any gas burners in the vicinity.

Fire extinguishers are available in various parts of the laboratory. For
burning oil use powdered sodium bicarbonate.

2. Burning Clothing: Avoid running (which fans the flame) and take great
care not to inhale the flame. Rolling on the floor is often the quickest and
best method for extinguishing a fire on one's own clothing. Smother the fire
as quickly as possible using wet towels, laboratory coats, heavy (fire)
blankets, or carbon dioxide extinguisher.

3. Treatment of Small Burns: Submerge the burned area in cold water until
the pain subsides. Blot the area dry, gently, with sterile gauze and apply a
dry gauze as a protective bandage. In small second or third degree burns in
which blisters have formed of broken, or in which deep burns are
encountered, see a physician as soon as possible.

4. Extensive Burns: These require special treatment to avoid serious or fatal

outcome---summon medical treatment at once. Combat the effects of shock
by keeping the patient warm and quiet.

Injuries and Chemical Burns

5. Reagents in the Eye: Wash immediately with a large amount of water,

using the ordinary sink hose, eye-wash fountain, or eye-wash bottle----do
not touch the eye.
After the eye has been washed thoroughly for 15 minutes, if any discomfort
remains, see physician.

6. Reagents on the Skin: Acids---Wash immediately with a large amount of

water, then soak the burned part in sodium bicarbonate solution. Cover the
burned area with a dressing bandage and see a physician.

Alkali---Wash immediately with a large amount of water, then soak the

burned area in 1% boric acid solution to neutralize the alkali. Cover the
burned area with a dressing and see a physician.

Bromine---Wash immediately with a large amount of water, then soak the

burned area with a dressing in 10% sodium thiosulphate, or cover with a
wet sodium thiosulphate dressing, for at least 3 hours and see a physician.

3
 Organic Substances---Most organic substances can be removed from the
skin by washing immediately with ordinary ethanol, followed by washing
with soap and warm water. If the skin is burned (as by phenol), soak the
injured part in water for at least 3 hours and see a physician.

7. Cuts: Wash the wound with sterile gauze, soap, and water. Cover with a
sterile dressing and keep dry.

WASTE DISPOSAL

IN AN EFFORT TO MINIMIZE THE AMOUNT OF HAZARDOUS WASTES

GENERATED IN ACADEMIC LABORATORIES CERTAIN PROCEDURES
HAVE BEEN INCORPORATED INTO THE EXPERIMENTS TO ACCOMPLISH
THIS.

1. THE SCALE OF THE EXPERIMENTS HAS BEEN REDUCED.

2. HAZARDOUS CHEMICALS HAVE BEEN REPLACED BY LESS

HAZARDOUS CHEMICALS

3. INSTRUCTIONS HAVE BEEN GIVEN FOR RECOVERING

CHEMICALS FOR RE-USE, WHENEVER PRACTICAL.

SPECIAL INSTRUCTIONS FOR THE DISPOSAL OF WASTES ARE PROVIDED

WITH THE EXPERIMENTS, WHERE NECESSARY.

SOLUTIONS ACCEPTABLE FOR SINK DISPOSAL SHOULD BE DILUTED

ONE HUNDREDFOLD BEFORE BEING SLOWLY POURED DOWN THE
DRAIN. ALTERNATIVELY THE SOLUTION MAY BE POURED DOWN
THE SINK ALONG WITH A STREAM OF WATER.

SMALL AMOUNTS OF WATER-SOLUBLE ORGANIC SOLVENTS MAY BE

DILUTED AND FLUSHED DOWN THE DRAIN.

WHEN IN DOUBT, CHECK WITH YOUR DEMONSTRATOR BEFORE

DISPOSING ANY CHEMICAL.

LARGE AMOUNTS OF ORGANIC SOLVENTS SHOULD BE PLACED IN

PROPERLY LABELLED BOTTLES FOR RECYCLING OR DISPOSAL.

BROKEN GLASS APPARATUS SHOULD BE PLACED IN SPECIALLY

DESIGNATED BINS FOR RECYCLING.

4
 POINTS FOR GRADING.
1. Ensure that you properly clean your workspace, the fume hoods and the centre
bench (which usually has the balances and communal reagents) at the end of the lab.
A majority of students forget the fume hood as well as the centre bench. However
significant marks in technique will be deducted if a clean work environment is not
maintained at the end of a lab session. If the fume hoods and centre bench are left in an
unclean state at the end of the laboratory session, marks will be deducted from the
entire class. Marks will also be deducted for leaving reagent bottles uncovered as well
as leaving your apparatus at the centre bench or fume hood. You thus have significant
control in maintaining your technique marks.

Remember that persons are not attracted to dirty Pharmacies!

2. Never begin any experiment unless you understand its overall purpose and reasons
for each operation involved in the experiment.

3. Always be neat and careful in handling chemicals, and in the assembly of apparatus.

4. Cultivate the habit of being observant during all stages of an experiment. (Was there
a fleeting colour change when a drop of reagent was added to the solution? Was a
precipitateformed? Is the reaction exothermic? Is your neighbour’s technique "better"
than your own?)

5. Record your observations and results in a bound notebook. Write in ink. Number
your pages of your notebook.

6. Your notebook should show the date and title of each experiment. Your report
should show the quantities of material used, the melting (or boiling) point of the
product obtained, the weight of the product and any other relevant data.

7. Your notebook should show each new experiment on a new page.

8. Save the final products from each experiment for examination by your
demonstrator.

9. When you have completed your lab, and properly cleaned your workstation, fume
hood and centre bench area, ensure that the lecturer (or
instructor/demonstrator/technician/lab assistant) signs your results. Also hand in a
single Master Copy of the lab results to the demonstrator.

5
MEASUREMENT OF MASS

Your Lecturer, demonstrator or technician will demonstrate the correct use of the
balances – top loading and analytical – and will help you understand the principles of
operation. The general rules to follow when making weighings are:
i. Use an assigned balance for all your determinations.
ii. Always level and zero balance before use.
iii. Consult an instructor if you need assistance.
iv. Clean up any spilled chemicals on balance immediately.
v. Leave the balance area free and clean of all chemicals, containers, paper etc.

MEASUREMENT OF VOLUME

The volume of a liquid can be measured easily and accurately by means of

specialized laboratory glassware called volumetric glassware: graduated cylinders,
volumetric flasks, pipettes, burettes. The proper use of glassware will be demonstrated
to you.

SEPARATION TECHNIQUES

Separation may be defined as an operation that results in the isolation and purification
of a single chemical constituent or phase. The process of separation may be divided
into two general categories depending upon the complexity of the method used. The
first category includes separation carried out by a mechanical operation such as
distillation, solvent extraction, sieving, centrifugation and filtration. The second
category of separations includes those carried out with the aid of chemical methods.

There are two kinds of filtration: GRAVITY FILTRATION

VACUUM FILTRATION

Vacuum filtration is more rapid and efficient than gravity filtration. In this technique
the filter paper rests flush against the flat bottom of a Buchner funnel. The funnel is
sealed to the top of a filtration flask by a rubber stopper or gasket ring. The sidearm of
the flask is connected to a water aspirator or vacuum line by heavy-walled tubing. This
connection is sometimes made through a "trap" jar to prevent the direct transfer of
liquids between the flask and the source of vacuum. The vacuum source greatly
reduces the presence in the filtration flask, causing the air pressure above the funnel to
push the mixture through the filter paper. The resulting force, causing the liquid to
pass through the filter paper, is much greater than the gravitational force used alone in
gravity filtration. The advantages are that large quantities of solid can be removed in
less time than by gravity alone.

6
 FUNDAMENTALS OF MEASUREMENT AND DATA EVALUATION

All measurements are subject to error. Experimental results are only as precise as the
measurements used to obtain them. Reported results should indicate the estimated
magnitude of the experimental error.

Experimental errors may be classified as belonging to one of the following three types:
1. Systematic errors result from faulty calibration of a measurement device.
Misapplication of a measurement technique, or use of an inappropriate
mathematical model. A meter stick might be 90 cm long yet still be divided into
100 cm units; the mass of an object might be read directly from a balance that has
not been previously zeroed; the area of a triangle might be incorrectly calculated as
the product of base times height. The effects of systematic errors are predictable
and correctable if the existence of the errors is recognized.

2. Random errors result from a large number of unknown and unpredictable

variations in measurement. They include the effects of observer judgements in
deciding when and how to read scales, temperature fluctuations, and mechanical
vibrations. Random errors often follow simple laws. The presence of random
errors can be detected and their effects minimized by replicate measurements.

3. Careless errors are made by the inattentive observer who misreads graduated
glassware, copies data incorrectly and makes mistakes in mathematical
calculations. These errors are totally avoidable and must be eliminated.

ACCURACY AND PRECISION

Precision and accuracy are two terms which have quite different meanings. The
precision of a measurement is the degree of agreement between it and other
measurements made under the same conditions. The accuracy of a measurement is
how closely it agrees with the accepted or true value.

The precision of a measurement is affected by random errors, which are caused by the
inability of a person to read and instrument accurately. The errors arise in the
interpolation between the scale divisions. The readings are either higher or lower than
the actual value. The precision of some instruments is given as follows:

0.02 mL for the 50 mL burette; 0.2 mL for the 50 mL graduated cylinder;

0.2° for the 110°C thermometer; 0.03 mL for the 25 mL transfer pipette;

0.2 mL for the 250 mL volumetric flask.

7
Results may have a high degree of precision without being accurate. But an accurate
result must be obtained from measurements made with high precision. Hence you
should strive for both precision and accuracy in the laboratory. In order to
illustrate this idea where three separate analyses were made by each of students A and
B on a sample containing 53.26% iron (Fe). Student A obtained values of 55.86, 55.92
and 55.89 or a mean value of 55.89% with average deviation of + 0.02% of the
measurements from the mean value. Student B obtained values of 53.09, 56.28 and
50.56 or a mean value of 53.31% with average deviation of + 1.98%.

From such data, student A's precision is high, but his average is by no means accurate.
Student B's average is very close to the true percentage, but precision is poor.
Therefore student B's result, though accurate, is NOT reliable.

SIGNIFICANT FIGURES

One method of indicating uncertainty is to include only significant figures or digits in

numerical expressions. Only the last digit in a number should be in doubt. Zeros are
assumed to be significant only when they are not needed in order to position the
decimal point. Table 1 includes numerous examples of determining the number of
significant figures in experimental data.

TABLE 1 Significant Figures (digits)

Measurement Significant Comments

Digits
5.630 4 Trailing 0 counted
0.270 3 Leading 0 not counted
1.0060 5 Each 0 counted
0.0004 1 Leading 0's place holders
-5002 4 _
8.1 x 107 2 first factor only
9.65 3 _
0856 3 leading 0 not counted
3 x 10 -6 1 first factor only
3600 2,3, or 4 0's may be holding decimal place
3.60 x 103 3 _

After all computations, the final answer should contain the proper number of
significant figures in order to express the degree of reliability of the result obtained.

In addition and subtraction, the last digit retained in the answer should correspond to
the first uncertain decimal place in any of the numbers. For example the sum of the
following numbers, namely, 32.7, 1.38, 0.423 is 34.5 (Since 32.7 + 1.4 + 0.4 = 34.5).

8
In rounding off numbers, increase the last digit by 1 if the digit which is to be
discarded is 5 or greater. If the rejected digit is less than 5, do not change the last
significant digit.

In multiplication and division, the answer should not have more significant figures in
any of the numbers entering into the computation. For example, the product of 0.112 x
14.73 x 23.169 is 38.1 (The number with the largest relative deviation is the first
number and the value is 1/112 times 100 = 0.9%. This means that the product can vary
by 9 parts per thousand or by 0.3 in 38.1).

ABSOLUTE AND RELATIVE ERRORS

In reporting the result of an experiment, the mean value or average of a number of

determinations is normally used, because it is more accurate than the individual
determinations.

The difference between the mean value obtained experimentally and the true value is
the absolute error. When this error is expressed in terms of percentage or parts per
thousand, it is called the relative error.

THE STUDENT MUST ALWAYS USE THESE CONCEPTS TO FACILITATE

HIS WORK

9
EXPERIMENT 1 STANDARDIZATION OF HYDROCHLORIC ACID
(USING SODIUM CARBONATE)

Objectives:

At the end of this session you should be familiar with the following:

i) The principles upon which volumetric analyses are based.

ii) The characteristics of primary standard solution.
iii) The mole concept.

Task:

In today's laboratory session you are required to perform the following:

1. Prepare a standard solution of anhydrous sodium carbonate.

2. Standardize a solution of hydrochloric acid using the sodium carbonate solution in
A.

A. Preparation of a Standard Solution of Sodium Carbonate

Procedure:

Weigh out accurately, approximately 1.3 g. of anhydrous sodium carbonate into a

volumetric flask (250 mL). To do this, first weigh out approximately 1.3 g of the
sodium carbonate in a sample bottle using the top loading balance provided. Then
using the analytical balance weigh accurately to four decimal places, sample bottle and
contents. Transfer quantitatively into volumetric flask by decanting small amounts of
sample from bottle into a funnel and washing carefully into flask with distilled water.
Shake to completely dissolve the sodium carbonate and then carefully make up to the
graduation mark with distilled water. Re-weigh sample bottle, record all mass in your
note-book and determine mass of sodium carbonate used by the method of difference.

10
Results

Mass of bottle and salt =

Mass of bottle =

Mass of salt =

B. Standardization of Hydrochloric Acid

Procedure:

Pipette 25 mL aliquots of the standard sodium carbonate solution prepared in Exercise

A above into conical flasks (250 mL). Titrate these samples with the hydrochloric acid
in the burette using methyl orange as indicator. Repeat until concordant results are
obtained. Record your results in tabular form in your note-book, as indicated below.

BURETTE ROUGH 1 11
READINGS
Final volume (mL)

Initial volume (mL)

Volume acid used

11
WORKSHOP SESSIONS

12
 PHARMACEUTICAL CALCULATIONS

The Properties of solutions: Measures of Concentration

I Normality and Molarity

A normal solution is one which contains one gramme-equivalent of the active

substance in 1000 mL. An equivalent (eq) in neutralization is the mass of acid that
yields 1 mol of H+ or the mass of base that reacts with 1 mol of H+

e.g. H2SO4 + 2NaOH  Na2SO4 + 2H2O

Each mole of H2SO4 supplies 2 mol of H+. Because the molar mass is 98.1g, an
equivalent of H2SO4 in this reaction equals 98.1g/2 = 49.0g. Because each mole of
NaOH reacts with 1 mole H+, an equivalent of NaOH = the molar mass (40.0g). One
eq of H2SO4 reacts with one eq of NaOH.

However, in the reaction

H2SO4 + NaOH  NaHSO4 + H2O

each mole H2SO4 supplies only 1 mol H+. Therefore an equivalent of H2SO4 in this
reaction equals the molar mass of 98.1g.

An equivalent (eq) in a redox reaction is the mass of oxidizing or reducing agent that
uses or provides one mole of electrons. Thus one eq of an oxidizing agent reacts with
one eq of reducing agent. For example the permanganate ion, MnO4- gains 5 electrons
when it is reduced to Mn2+ in acidic solution

MnO4- + 8H+ + 5e  Mn2+ + 4H20

An eq of KMnO4 is obtained by dividing its molar mass (158.0g) by the number of

electrons gained (5), i.e. 158.0g/5 = 31.6g
The Normality of a solution is the number of equivalents of a substance dissolved in a
litre of solution. It equals the molarity of the solution times the number of equivalents
per mole. For example, if the reaction is an oxidation by KMnO4 in acidic solution, the
normality of 0.10 M KMnO4 is

Normality = moles of substance equivalents substance

Litres solution X moles substance
M

= 0.1 mol KMnO4 X 5 eq KmnO4

L solution mol KmnO4

= 0.50 N KMnO4

13
A molar solution (designated M) is one which contains the gram-molecular weight of
the substance in one litre of solution. The strengths of molar solutions are independent
of the reaction under consideration.

II Volume percent composition and mass percent composition

Volume percent composition

Many solutions are prepared by measuring the volume of a solute, instead of by its
mass, and mixing it with the solvent. A convenient expression of the resulting
composition is in terms of the volume percent composition., the volume of a substance
present in a solution expressed as a percentage of the total volume. Volume percent is
the basis of the measurement of alcohol (ethanol) content of beers, wines and spirits. A
typical wine has about 15% by volume alcohol (i.e. 100 mL wine contains 15 mL
ethanol). The proof scale equates 100 proof with 50% by volume ethanol.

When there is only a small quantity of solute in a solution, and particularly when the
solution is gaseous (e.g. a pollutant in air) the composition is often expressed in parts
per million by volume (ppm by volume) , which is 106 times the ratio of the volume of
the solute to the volume of the sample. It follows that parts per million by volume is
numerically equal to the volume percentage composition multiplied by 104. Thus a
SO2 concentration expressed as 42 ppm by volume would correspond to 42 mL of SO2
in a sample of volume 103 L.

Mass percentage composition

The mass of one substance present in a mixture expressed as a percentage of the total
mass:

Mass percentage of A = mass of A in solution X 100%

total mass of solution

= mA
__________ X 100%
mA+mB+…

This measure is often used when reporting the composition of a solution of a solid
solute. For example, we may report the composition of a solution of sucrose in water
as being 22.1% by mass of sucrose. When the mass of solute is very small, a widely
used measure of composition is parts per million by mass (ppm by mass). For the
analysis of pollutants in water, part per million is 106 times the ratio of the mass of the

14
solute to the mass of the sample. In practice it is the mass of solute in milligrams per
kilogram of sample (mg/kg).

III Mole Fraction and Molarity

The mole fraction, x, of a species in a mixture is the number of moles of that species
expressed as a fraction of the total number of moles of ions and molecules in the
mixture.

For solute molecules in a nonelectrolyte solution, mole fraction is

xsolute = nsolute
________

nsolvent + nsolute

where nsolute is the number (in moles) of a solute present and nsolvent, the amount (in
moles) of solvent. A similar equation defines the mole fraction of the solvent
molecules xsolvent . A useful relation between the two is
nsolvent + nsolute
xsolvent + xsolute = ________ ________ = 1

nsolvent + nsolvent nsolvent + nsolute

A mole fraction must lie in the range xsolute = 0 (no solute) to xsolute = 1 (pure solute).

For an electrolyte solution, the mole fraction is calculated by treating the cations and
anions as individual particles: hence

ncations
xcations = ___________________
nsolvent + nsolvent + nanions

IV Molality

The molality of a solution also emphasizes the relative numbers of solute and solvent
molecules. The molality of a solution is the amount of solute per kilogram of solvent:

Molality = amount (mol) of solute

mass (kg) of solvent

15
The units of molality, moles per kilogram of solvent (mol/kg), are often abbreviated as
m and read “molal”. The emphasis on solvent in the definition should be noted. It
means that to prepare a 1 m NiSO4 (aq) solution, 1 mol of NiSO4 is dissolved in 1 kg
of water. Because 1 kg of solvent consists of a definite number of moles of molecules
(55.5 mol H2O per kilogram of water), the higher the molality of a given solution, the
higher the proportion of solute molecules.

The molality is a conversion factor from the mass of solvent in a sample to the number
of moles of solute in it:

amount of solute (mol) = mass of solvent (kg) x amount (mol) of solute

mass (kg) of solvent

The molality of a solution must be carefully distinguished from its molarity (its molar
concentration). The molality is the moles of solute per kilogram of solvent. The molar
concentration is the moles of solute per liter of solution. There are two good reasons
for introducing molality in addition to molar concentration. One is that the molality
makes it very easy to calculate the relative numbers of solute and solvent molecules in
a solution. The second is the molality is independent of temperature, whereas the
molar concentration is not (because the volume of the solution increases as the
temperature is raised).

The relation between the volume of a solution and the mass of solvent present in it is
obtained by using the density of the solution(to obtain the total mass of the solution),
the mass of solute (which is known from the molar concentration and the molar mass
of the solute), and the relation

mass of solution = mass(solvent) + mass(solute)

to obtain the mass of solvent.

V Percentage Concentrations

Before we use mole fractions or molalities in a study of certain physical properties of

solutions, we will complete the list of the chief ways by which chemists describe
concentrations. The rest of the list are various kinds of percent concentrations.

In most chemical laboratories, a percent concentration means percent by weight or

weight/weight percent. The symbol for it is usually % (w/w). This is the number of
grams of solute per 100 grams of solution (not solvent). A solution labeled “0.9%
(w/w) NaCl”, for example, is one in which the ratio of solute to solution is 0.9g of
NaCl to 100g of solution.

16
EXAMPLES

USING WEIGHT/WEIGHT PERCENTS

Problem How many grams of a 4.00% (w/v) solution of NaCl is needed to obtain
0.500 g of NaCl?

Solution The given concentration gives us the following conversion factors:

4.00 g NaCl 100 g solution

and
100 g solution 4.00 g NaCl

We want 0.500 g of NaCl from this solution, so we use the second

conversion factor.

100 g solution
0.500 g NaCl X = 12.5 g of 4.00% (w/w) solution
4.00 g NaCl

Thus if we take 12.5 g of the 4.00% (w/w) NaCl solution we will also
be taking 0.500 g of NaCl.

PREPARING WEIGHT/WEIGHT PERCENT SOLUTIONS

Problem “White vinegar” can be made by preparing a 5.0% (w/w) solution of

acetic acid in water. How would you make 500 g of such a solution?

Solution The mass of acetic acid first has to be calculated. Then it has to be
combined with enough water to make the total solution have a mass of
500 g. To find the mass of solute, we use the given concentration to
give us our choice of conversion factors. Thus, 5.0% (w/w) acetic acid
means:

5.00 g acetic acid 100 g solution

and
100 g solution 5.00 g acetic acid

We have to use the first factor to get the units to work out.

5.0 g acetic acid

500 g solution X = 25 g acetic acid
100 g solution

17
 Thus if we dissolve 25 g acetic acid in enough water to make
the final mass equal to 500 g , we would have a 5.0% (w/w)
solution of acetic acid – the same as white vinegar. This, of
course, would require 475 g of water (500 g –25 g).

NOTE More than two-significant-figure precision is not often

sought when solutions are made up to a percent
concentration.

Because we know that the density of water at room temperature is (to two significant
figures) 1.0 g/mL, we can easily see that 475 g of water needed in this example is the
same as 475 mL of water. When greater precision is not needed, a chemist will
generally make this mental calculation and then mix 25 g of acetic acid with 475 mL
of water to make the 5.0% (w/w) acetic acid solution. It is just easier to measure a
large volume than a large mass because large graduated cylinders are readily available.

When both solute and solvent are liquids, or both gases, then it can be converted to use
percent by volume – symbolized as % (v/v) – which is the number of volumes of one
component in 100 volumes of the entire solution. (Notice again that the emphasis is on
the volume of the final solution.) The unit of volume can be any unit, provided that the
same unit is used for both solute and solution. (True percentages, of course, have no
formal units because they cancel in the final calculation, but we still have to remember
how each kind of percent concentration is defined.)

USING VOLUME/VOLUME PERCENTS

Problem A 40% (v/v) solution of ethylene glycol in water gives an antifreeze

that will protect a vehicle’s cooling system to -24C (-12F). What
volume of ethylene glycol has to be used to make 5 quarts of this
solution?

Solution First, we use the given concentration to construct conversion factors.

Thus, “40% (v/v) ethylene glycol ” means:

40 vol ethylene glycol 100 vol solution

and
100 vol solution 40 vol ethylene glycol

We have to use the first factor to get the answer in units of ethylene
glycol. And we substitute “quarts” for “vol” now.

40 quarts ethylene glycol

5 quarts solution X = 2 quarts ethylene glycol
100 quarts solution

18
 Thus if we dissolve 2 quarts of ethylene glycol in enough water to make
the final volume of the solution 5 quarts, the antifreeze will be 40%
(v/v) ethylene glycol. (Incidentally, we could not assume that all we
had to do was add 2 quarts of ethylene glycol to 3 quarts of water to
make 5 quarts of solution. When two liquids mix, the final volume is
sometimes less than the sum of their initial volumes, and sometimes
more. Sometimes it is the same, but this cannot be assumed. It depends
on how the individual molecules find room for each other in the
solutions.)

Some fields of science employ still other kinds of percent concentrations, but
they are not true percents (the units do not easily cancel) and they are not
preferred by chemists. In case you might run into them we have described a
few in the Special Topic.

SPECIAL TOPIC: SOME HYBRID PERCENT CONCENTRATIONS

By “hybrid percent concentration” we mean one in which the units do not cancel. For
example, a weight/volume percent concentration gives the grams of solute in 100
mL of solution. When the solvent is water and the solution is dilute, the numerical
value of a weight/volume percent concentration is virtually the same as that of a
weight/weight percent.

People in the health fields sometimes use a milligram percent concentration, which
gives the number of milligrams of solute in 100 mL of solvent.
Whenever a percent concentration is given without any specification about its type,
assume that it means a weight/weight percent.

CONVERTING AMONG CONCENTRATION UNITS

Many made-up solutions are available from chemical supply houses and stockrooms,
as you have probably already seen in the lab. Sometimes in working with a solution
whose molarity is known we run into a situation where we would like to know its
molarity or its percent (w/w) concentration, too. Is there any way we can calculate one
kind of concentration from another?

The only additional information we need for some calculations are formula weights
and densities, which are often given in tables in reference handbooks for chemistry.
These conversions are easy, provided you know the definitions of each kind of
concentration and can prepare conversion factors from given concentrations. In fact,
working through these examples and doing practice exercises is a superb way to get a
final and lasting grasp of all the concentration expressions.

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EXAMPLES

CONVERTING FROM WEIGHT PERCENT TO MOLE FRACTIONS

Problem What are the mole fractions and mole percents of the components in
10.0% (w/w) NaCl, the same solution we used in the previous example?

Solution Our goal is to move the units from those of percent (w/w),

g solute

100 g solution

to those implied by a mole fraction,

mol solute

total moles

CONVERTING FROM WEIGHT PERCENT TO MOLALITY

Problem What is the molality of a 10.0% (w/w) NaCl solution?

Solution We are given a ratio of 10.0 g of NaCl to 100 g of solution. This is what
the percent (w/w) means. But the units of molality are

mol of solute
kg of solvent

What we need to do, then, is use the units of the percent concentration
to work out the units of molality. The steps are

Step 1. Calculate the moles of NaCl in 10.0 g of NaCl.

Step 2. Calculate the kilograms of H2O in 100 g of this solution.
(Remember it is grams of solution with percent concentrations,
but kilograms (or1000 g) of solvent with molality.)
Step 3. Calculate the ratio of these, because molaltiy is the ratio of
moles of solute to kilograms of solvent.

We find the moles of NaCl in 10.0 g of NaCl in the usual way, using
the molar mass of NaCl, 58.5 g NaCl/mol NaCl.

1 mol NaCl
10.0 g NaCl X = 0.171 mol NaCl
58.5 g NaCl

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 Next, step 2, we note that 100 g of this solution, which has 10.0 g of
solute, must therefore have 90.0 g of solvent (100 g – 10 g). So the
kilograms of solvent are found by

1 kg H2O
90.0 g H2O X = 0.0900 kg H2O
1000 g H2O
Remember, both numbers in 1 kg = 1000 g are defined as exact.

Finally, step 3, we calculate m, the ratio of moles of solute to kilograms

of solvent.

0.171 mol NaCl

= 1.90 m
0.0900 kg H2O

Thus, 10.0% (w/w) NaCl is also 1.90 m NaCl.

The amount of solute from the previous example is 0.171 mol of NaCl. We also found
in that example that there is 90.0 g H2O in 100 g of solution. And the moles of water in
90.0 g of H2O (at 18.0 g H2O/mol H2O) is

1 kg H2O
90.0 g H2O X = 5.0 mol H2O
18.0g H2O

So the total number of moles of both solute and solvent in 10.o% (w/w) NaCl is

0.171 mol + 5.0 mol = 5.17 mol (correctly rounded)

Now we can calculate mole fractions of solute and solvent.

For NaCl

XNaCl = 0.171 mol = 0.0331 (or 3.31 mole percent)

5.17 mol
For H2O

XH2O = 5.00 mol = 0.967 (or 96.7 mole percent)

5.17 mol

For a two component system like this, we would not need this last calculation. The
mole fractions must add up to 1 (or the percents, to 100%), so we could have found the
mole fraction of water simply by subtracting the mole fraction of NaCl from 1.00. (Or
we could have calculated the mole percent of water by subtracting the mole percent of
NaCl from 100.)

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CALCULATING PERCENTS BY WEIGHT FROM MOLE FRACTIONS

Problem So-called “100 proof” alcohol has the following mole fractions of
components: for water 0.765, and for ethyl alcohol, 0.235. Calculate the
percents (w/w) of water and ethyl alcohol in 100 proof ethyl alcohol.
The formula weights are: H2O, 18.0; and ethyl alcohol, C2H5OH, 46.1.

Solution As in all kinds of calculations, we work from the meanings of the given
concentration units toward the final units. To work toward percents by
weight, we have to work toward a ratio calculated from grams of
components. Let us start with water. When the mole fraction of water is
0.765, we know that there are 0.765 mol of H2O in a total of 1.00 mol
of all components. So, in terms of grams of water, at 18.0 g H2O/mol
H2O, we have

18.0 g H2O
0.765 mol H2O X = 13.8 g H2O
1 mol H2O

Next, we take ethyl alcohol. When its mole fraction is 0.235, we know
that there is 0.235 mol of C2H5OH in 1.00 mol of all its components.
So, in terms of grams of C2H5OH, at 46.1 g C2H5OH/mol C2H5OH, we
have

46.1 g C2H5OH
0.235 mol C2H5OH X = 10.8 g C2H5OH
1 mol C2H5OH

Thus, in “1.00 mol” of this ethyl alcohol solution there are 13.8 g of
H2O and 10.8 g of C2H5OH. To convert to percents by weight, we need
the total mass of the solution, which is 13.8 g + 10.8 g = 24.6 g. For the
13.8 g of water, its percentage of 24.6 g is

13.8 g
X 100 = 56.1% (w/w)
24.6 g

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 APPENDIX I

CONCENTRATIONS OF COMMERCIAL REAGENTS

Concentrated hydrochloric acid 1.19 g cm-3is 12 M

Concentrated nitric acid 1.42 g cm-3is 16 M

Concentrated sulphuric acid 1.84 g cm-3is 18 M

Glacial acetic acid 1.05 g cm-3is 17 M

'0.880' ammonia 0.88 g cm-3is 15 M

'20 volume' hydrogen peroxide (fresh) is approx. 1.8 M

Fresh sodium hypochlorite (15% w/v) is approx. 2M

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 APPENDIX 11

Relative Atomic Weights ( 12 C=12 )

ELEMENT SYMBOL ATOMIC ATOMIC

NUMBER WEIGHT

Bromine Br 35 79.9
Calcium Ca 20 40.08
Carbon C 6 12.01
Cerium Ce 58 140.12
Chlorine Cl 17 35.45
Chromium Cr 24 51.99
Copper Cu 29 63.54
Fluorine F 9 18.99
Hydrogen H 1 1.01
Iodine I 53 114.82
Iron Fe 26 55.85
Lead Pb 82 207.19
Magnesium Mg 12 24.31
Nitrogen N 7 14.01
Oxygen O 8 15.99
Phosphorus P 15 30.97
Potassium K 19 39.1
Silver Ag 47 107.87
Sodium Na 11 22.99
Sulfur S 16 32.06
Thallium Tl 81 204.37
Tin Sn 50 118.69
Zinc Zn 30 65.370

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 APPENDIX III

BIBLIOGRAPHY

Beckett, A.H. and Stenlake. Practical Pharmaceutical Chemistry, Third Edition :

Part 1

Bentley and Driver. Textbook of Pharmaceutical Chemistry, Eight Edition

Education in Chemistry (bimonthly)

Hunt, H.R. and Block, T.F. Laboratory Experiments for General Chemistry

Journal of Chemical Education (monthly)

Masterton, W.L. and Hurley, C.N. Principles and reactions, Second Edition.

Milio, F.R. ; Debye, N.W.G. ; Metz, C. Experiments In General Chemistry

U.W.I. Department of Chemistry C10 Laboratory Course

Vogel, A.I. "A Textbook of Macro and Semimicro Qualitative Inorganic Analysis"
(Longmans).

Vogel, A.I. "A Textbook of quantitative Inorganic Analysis" (Longmans).

Vogel, A.I. "Elementary Practical Organic Chemistry" (Longmans).

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