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CHAPTER 1

(INTRODUCTION: ANALYTICAL
CHEMISTRY)

Lesson Outcomes:
Differentiate between qualitative & quantitative
analysis
Explain the steps involve in quantitative analysis
Calculate the concentration of solution
Explain the preparation of solution

Importance of Analytical Chemistry


Analytical chemistry is applied throughout industry,
medicine and all the sciences.
Analytical chemistry is used to collect necessary data
to solve problems in many fields of science such as:
Chemistry,
Biology,
Environmental
Studies,
Agriculture,
Medicine,
Materials
Science,
Archeology, Forensic Science, Geology, Physics,
Engineering, etc

Methods of Chemical Analysis


To estimate the concentration of an analyte may require
both measurement of the mass or volume of the sample
and some physical quantity that is related to the
concentration of the element or compound
This quantity can be classified as:
1. Gravimetric - mass of a precipitate
2. Volumetric - volume of a titration
3. Electroanalytical - voltage, current, amount of charge
4. Spectroscopic - absorbance, fluorescence, emission
5. Miscellaneous - radioactivity, reaction rate, refractive
index

Types of Analysis
Analytical chemists perform two main tasks:
Qualitative

Quantitative

To detect the presence of a


substance in the sample

To indicate the amount of


each substance in a sample

Finding out what


substances

Finding the amount


(quantity) of substances

Steps in Analysis
Defining the problem

Selecting the method


Acquiring the sample
Processing the sample
(Preparing Sample for analysis)

Eliminating interferences
Performing the Measurement

Calculating and Presenting the Results

1. Defining Problems
The goal of every chemical analysis is to obtain the
required information within a period of time
acceptable to the customer.
Many problem do not require complete
identification and many cases require only a general
classification.
It is important for the analyst to determine the
information required by the client.
For example, in water analysis, only the total
hardness is required rather than the concentration
of individual Ca2+ and Mg2+ ion concentration is not
necessary.

2. Selecting the Method


Literature search is essential to find an appropriate
procedures
Patents or commercial literature usually help in
determination of the composition of industrial
materials.
Others:
- book
- review articles/journal
- standard organization :
i) Association of official Analytical Chemists (AOAC)
ii) Food and Drug Administration (FDA)
- electronic media

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Questions to be considered:
What is the concentration range (detection limit)
What accuracy is required (depends on the
problem)
What elements or compounds are involved
How complex is the mixture (selectivity,
separation)
How many samples are involved (analysis time)
What methods are available to you !!!

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3. Acquiring the Sample (Sampling)


Sampling: Process of selecting representative
material from the lot and storing the sample
Chemical analysis usually performed on only a small
portion of the material
If the amount of material is very small and it is not
needed for future use, the entire sample may be
used for analysis
The suitable sampling method differ from one
substance to another depending on homogeneity

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Homogeneous: Substance that has the same


composition throughout the sample
Heterogenous: Substance that has different
composition from one reagent to another reagent
Proper procedure must be used to store both
samples and standards
All sample must be properly labeled and recorded

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4. Processing the Sample


Preparing and storing samples:
- SOLIDS - grinding, mixing, storage to avoid
changes (water content, oxidation). Selecting the
subsamples for analysis
- LIQUIDS solvent & analyte evaporation,
settling of solids, storage to minimise chemical
changes (refrigeration, freezing, deoxygenate,
dark)
Preparing Solutions how to dissolve the sample ?
(acid, base, oxidant, reductant, organic solvent)

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Steps of sample preparation involved


bulk materials:
Bulk sample must be reduced in size to obtain a
laboratory sample of several grams.
Only a few grams to milligrams will be taken to be
analyzed (analysis sample).
The size reduction may require taking portions (two
quarters) and mixing, in several steps, as well as
crushing and sieving to obtain a uniform powder for
analysis.

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5. Eliminating Interferences
Impurities may contribute to (or decrease) the
spectroscopic signal used to calculate the
concentration e.g. Si produces the same blue colour
as PO43- with molybdenate reagent
These interferences must be identified and their
effect eliminated which can present a difficult
problem

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Why sample pretreatment is


important?
Laboratory samples are often subjected to physical
or chemical pretreatment where it is converted to a
form that is suitable for the measurement.

During pretreatment:
reduce and remove interferences
adjust analyte concentrations to a range suitable for
measurement
produce species from analyte that have
quantitatively measurable properties

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6. Performing the Measurement


Analysis: Incorporates the measurement of the
concentration of the analyte in replicates and
comparing with standards
Replicate measurement: the practice of taking
multiple readings
The replicate measurements are necessary to obtain
the measurement uncertainty
The uncertainty important as it indicates the
reliability of the measurements

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7. Calculating and Presenting the


Results
Statistical analysis (eg. Standard deviation)
Deliver a clearly written, complete report and
their limitations.
Analyst should critically evaluate whether the
results are reasonable and relate to the analytical
problem.

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Moles & Milimoles


One mole (mol) is the amount of a substance that
contains as many entities (atoms, molecules or ions)
as there are in 12.0 g of C-12 atoms.
The mass in grams of 1 mole of a substance is called
its molar mass.
1 mole of atoms/molecules/ions of any element will
contain
Avogadros
number
of
atoms/molecules/ions
or
6.02
x
1023
atoms/molecules/ions of that element.

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Moles =
grams
formula weight (g/mol)

Milimoles =
miligrams
formula weight (mg/mmol)
1 mole = 1000 milimoles
Sometimes it is more convenient to make calculations
with milimoles (mmol) rather than moles, where the
1 milimole = 0.001 mole

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Example:
Calculate the number of moles in 500 mg Na2WO4
Solution:
Moles =

grams
formula weight

500 mg/1000

293.8
= 0.0017 mol

1 g = 1000 mg

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Example:
How many mg are in 0.250 mmol Fe2O3?
Solution:

Milimoles =

miligrams
formula weight (mg/mmol)

Miligrams = milimoles x formula weight


= 0.250 mmol x 159.7 mg/mmol
= 39.9 mg

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Example:
How many moles and milimoles of benzoic acid
(Molar mass =122.1 g/mol) are contained in 2g of
pure acid?

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Solution:
Mole = mass (g)/molar mass (g/mol)
= 2g of benzoic acid x 1 mol benzoic acid
122.1 g benzoic acid
1 mole = 1000
= 0.0164 mol benzoic acid
milimole
Milimole benzoic acid

So, 0.0164 x 1000


= 16.4 milimole

= mass (mg)/molar mass (mg/mmol)


=122.1g of benzoic acid
x 1000 mg x
1 mol
1 mol benzoic acid
1g
1000 mmol
= 122.1 mg/mmol
So, 2000 mg of benzoic acid x 1 mmol benzoic acid
122.1 mg benzoic acid
= 16.4 mmol benzoic acid

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Exercises:
1. Calculate the number of moles for 3.4 g of carbon
atoms.
2. What is the mass of 0.30 moles of CH4?
3. How many moles of Cl- is present in 0.34 moles of
CaCl2?
4. What is the mass of H in 2.5 moles of H2O?
5. What is the mass of O in 3.0 moles of CO2?

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What is solution concentration?


Concentration is the amount of solute in a given
volume of solution
Solution: A homogenous mixture of two or more
substances, consisting of solvent and solute
Solute: The substance present in a smaller
proportion of the solution. It can be solid, liquid or
gas.
Solvent: A substance that generally a liquid
present in the larger proportion of the solution
Water is considered a universal solvent for most
solutions

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How do we express concentrations of


solution?
Molarity (M) : No of moles of the solute in 1L of
solution
M = no.mol solute (mol)
L solution

Molality (m) : No of moles of the substance per


kilograms of the solvent
m = no.mol solute (mol)
kg solution

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Density Calculations How do we


convert to molarity?
Density - the mass of the solution per a unit of
volume
Density of a solution correlates with the
concentration of the dissolved substance
Molarity is the most common way to express the
solution concentration that reports the number of
moles of the dissolved compound (solute) in 1 liters
(L) the solution.

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Example:
What is the molarity of a solution of 0.60 g NaCl in
100 mL of solution? Given, MW NaCl = 58.5 g/mol
Solution:
No. of mol =

0.60 g
58.5 g/mol
= 0.0102 mol

Molarity

= 0.0102 mol
0.1 L
= 0.102 M

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Example:
If you have 10.0 grams of Br2 and dissolve it in 1.00 L of
cyclohexane, what is the molality of the solution? The
density of cyclohexane is 0.779 kg/l at room
temperature.
Solution:
Mole of Br2
10 g / (159.8 g/mole) = 0.063 moles Br2
Convert the volume of solvent to the weight of solvent
using the density
1.00 L x 0.779 kg/l = 0.779 kg
Divide the two to get the molality 0.063 moles Br2/ 0.779
kg cyclohexane
= 0.080 molal

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Example:
Calculate the molarity of a potassium hydroxide
(KOH) solution having a density of 1.28 g/mL and
containing 25 percent (by weight) of the dissolved
compound.

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Solution:

Formula weight of KOH = 39 + 16 + 1 = 56 g/mole

Multiply the solution density by 1000 to calculate the


weight of 1000 ml (1 L) of the solution.
1.28 g/ml x 1000 ml = 1280 g

Multiply the mass from Step 2 by the mass percentage of


the solute, and then divide by 100 to compute the mass of
the dissolved compound in 1L of the solution.
The mass of KOH is 1280 g x 25/100 = 320 g
Divide the mass of the dissolved compound in 1L of the
solution by its molecular mass to calculate the molarity of
the solution
The molarity is
320 g
= 5.71 M
56 (g/mole)

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Example:
As a student, you are given copper (II) sulphate pentahydrate
(CuSO4.5H2O, MW 249.69 gmol-1). Describe how you can
prepare a 500 mL standard solution of 10.00 mM Cu2+ from
the reagent.

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Exercise:
How many milliliters of concentrated sulfuric acid,
94.0% (g/100 g solution), density 1.831 g/cm3, are
required to prepare 1 L of 0.100 M solution?

Answer: 5.71 mL

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Other Representations of
Concentration
Percent Concentration:
Weight % (w/w) = Weight solute (g)
x 100
Weight of solution (g)
Volume % (v/v) = Volume solute (mL) x 100
Volume of solution (mL)

Weight/Volume = Weight solute (g)


x 100
% (w/v)
Volume of solution (mL)

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w/w % is frequently used to express


concentration of commercial aqueous reagents

the

v/v % is commonly used to specify the concentration


of a solution prepared by diluting a pure solute with
another liquid
w/v % is often used to indicate the composition of
dilute aqueous solutions of solid reagents

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Example:
Briefly explain how to prepare 1.0 L 10.50% (w/v)
aqueous CH3CH2CH2OH
Solution:
%w/v =

weight solute (g)


x 100
volume sample (mL)

10.50 = weight solute x 100 = 105 g


1000
Step of preparation:
1.
Weight a certain quantity of the solid reagent
2.
Dissolve it in a solvent in a volumetric flask.

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For a very dilute solutions:


ppm = parts per million (106)
ppb = parts per billion (109)
ppt = part per trillion (1012)
parts of a substance present in one million (or 1
billion) parts of solvent (water)
If we use gram as the unit, 1ppm means we have 1 g
of substance in 1,000,000 g solvent.

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For dilute aqueous solutions whose densities are


approximately 1.00 g/mL, 1 ppm=1.00 mg/L
C ppm =

mass solute (mg)


volume solution (L)

C ppb = mass solute (g) x 109


mass solution (g)

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Common unit to express content


Expression Abbreviation

Parts per
million

Parts per
billion

ppm

ppb

Units
w/w

w/v

v/v

g/g

g/mL

nL/mL

mg/kg

mg/L

L/L

ng/g

ng/mL

nL/L

g/kg

g/L

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Example:
What is the molarity of K+ in a solution that
contains 63.3 ppm of K3Fe(CN)6 (329.3 g/mol)?

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Solution:
Because the solution is so dilute, assume its density = 1.00
g/mL. So,
63.3 ppm K3Fe(CN)6 = 63.3 mg K3Fe(CN)6 /L

[K3Fe(CN)6] = 63.3 mg K3Fe(CN)6 x 1 g K3Fe(CN)6


L
1000 mg K3Fe(CN)6
x 1 mol K3Fe(CN)6
329.3 g K3Fe(CN)6
= 1.922x10-4 mol/L @ M
[K+] = 1.922x10-4 mol K3Fe(CN)6 x
3 mol K+
L
1 mol K3Fe(CN)6
= 5.77x10-4 mol K+/L @ M

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Exercise:
250 mL 50 ppm of Ca2+ from the solid chemical
Ca(NO3)2

Answer: 0.0513 g

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Dilution
Dilute solution (with low concentration) can be
prepared from a more concentrated solution
A known volume of the concentrated solution
can be transferred into a new flask and diluted to
the required volume or weight

M1V1 = M2V2

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Example:
The laboratory grade concentrated HCl has a
concentration of 12.1 M. What a volume of the
concentrated acid is necessary to prepare 500 mL of 0.100
M HCl?

Solution:
M1V1 = M2V2
(12.1 M) x V1 = (0.100 M) x 500 mL
V1 = (50.0) / 12.1 = 4.13 mL.
Procedures:
1. Dilute 4.13 mL of concentrated acid in a 500-mL VF
2.Dilute with distilled water to the 500-mL mark
3.Invert the flask several times to ensure complete mixing.