CHAPTER 1:

INTRODUCTION OF ANALYTICAL CHEMISTRY

 SYLLABUS CONTENT
 Types and steps in analysis.
 Review the terms: moles, molarity and concentration.
 Other expressions of concentration: % (w/w), %
(w/v),
% (v/v), ppm, ppt, ppb.
 Calculations involving different expressions of
concentrations.
 LEARNING OUTCOME

 In this chapter, student should be able to:

 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
 Measurement and characterization of a chemical
species that contain in a sample.
 Provide methods and tools to collect data to solve
problems in FIELDS OF SCIENCE such as:
 Industry, Medicine, Environment, Chemistry, Biology,
Agriculture, Materials Science, Archeology, Forensic
Science, Geology, Physics, Engineering and more.
 In analysis, QUALITATIVE & QUANTITATIVE
information are required.
1. TYPE & STEPS IN ANALYSIS
DISCIPLINE OF ANALYTICAL CHEMISTRY

ANALYTICAL CHEMISTRY

QUALITATIVE QUANTITATIVE
ANALYSIS ANALYSIS

To identify the components To determines the relative amounts

(elements, atoms, ions & of the components presence in a
compounds) present in a sample. sample.

WHAT IT IS? HOW MUCH?


QUALITATIVE vs QUANTITATIVE
QUALITATIVE
To determine the PRESENCE or
ABSENCE of a substance in a sample
CHEMICAL IDENTITY of the substance
of the sample.
(Type of species/analyte/atom/ion/
molecule/functional group present)
Eg:
1. The presence of copper ion
detected when flame colour is
green (Flame Test)
2. Identifying anions and cations in
aqueous solution
Achieved by:
• Color changes, distillation,
extraction
• Gravimetry: precipitation
• Chromatography: separation
ANALYTE:
components in a
sample that are
to be
determined
QUANTITATIVE
To determine the EXACT AMOUNT of that
substance/analyte in a sample
QUANTITY of the species in a sample.
(Concentration/level/percentage/mass/rel
ative abundance)
Eg:
1. The concentrations of oxygen in blood
samples is equal to 3 mL O2/liter blood.
2. The percentage by mass of silver is
42.88% in ore.
Achieved by:
• Adsorption of light, density, chemical
reactions, precipitation
• Volumetric: Titration
 METHOD 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:

 Gravimetric [mass of a precipitate]
 Volumetric [volume of a titration]
 Electroanalytical [voltage, current, amount of charge]
 Spectroscopic [absorbance, fluorescence, emission]
 Miscellaneous [radioactivity, reaction rate, refractive index]
 EXERCISES
State the types of analysis: qualitative analysis,
quantitative analysis or both.
a. To determine and compare the percentage yield of fish oil in siakap and
tilapia fish
b. To determine the presence of ascorbic acid in canned fruit juices
c. To determine the amount of potassium content in varieties of local
durians.
d. A hazardous-waste disposal site is believed to be leaking contaminants
into the local groundwater.
e. A quick way is needed to find the level of blood pressure among men
above 60 years old that can categorized as high BP.
f. A reliable method is needed by airport security for detecting the
presence of explosive materials in luggage.
 STEPS IN ANALYTICAL CHEMISTRY
Defining the problem

Selecting the method

Obtain a representative sample

Prepare the sample for analysis

Eliminating interferences

Performing the measurements

Calculating the results and reporting the data

 STEP 1 DEFINING THE PROBLEM

 To obtain required information within a period of time

 Know what information is needed, by whom, what

purpose & what type of sample is to be analyzed.
 Depend on equipment available, cost, time involved.
 STEP 2 SELECT A METHOD

 Factors to select a method:

• Sample type
• Size of sample
• Level accuracy
• Sample preparation needed
• Transportation or storage of sample

 Complexity of sample & no. of components

in sample influence the choice of method applied.
 OBTAIN A REPRESENTATIVE
STEP 3
SAMPLE
 Representative sample: A small quantity/portion of materials
that represent the whole sample of population

 Sample (Solid/Liquid/Gas) may be homogeneous or

heterogeneous.

 Gross sample:
• consist several portions of tested material
• must be reduced in size to gain laboratory sample

 Laboratory sample:
• small portion, crushing or sieving to form homogeneous or
uniform powder for analysis
• the analysis sample that actually analyzed
 STEP 4 PREPARE THE SAMPLE FOR
ANALYSIS
 Preparing laboratory samples
 SOLIDS : grinding, mixing, storage to avoid changes
(water content, oxidation).
 LIQUIDS : solvent & analyte evaporation, storage to
minimize chemical changes (refrigeration,
freezing, deoxygenate, dark).

 Replicates samples
 Improve the quality of the results & provide a measure
reliability.

 Preparing and storage the solutions

 Physical & chemical changes can occur
 know suitable solvent used (acid, base, oxidant,
reductant, organic solvent)
 STEP 5 ELIMINATING INTERFERENCES

Perform necessary chemical separation to

remove interference

 Impurities may decrease the spectroscopic signal used

to calculate the concentration.
 Separation step include precipitation, extraction,
chromatography, distillation.

INTERFERENCE
Species other than analyte that can cause ERROR
& affect the final measurement
 STEP 6 PERFORMING THE MEASUREMENTS

 Gravimetric analysis
Involve separation of analyte by
precipitation followed by MEASUREMENT OF
MASS.

 Volumetric analysis
 Analyte reacts with a measured volume of reagent
of known concentration, in a process called
titration.
 STEP 6 PERFORMING THE MEASUREMENTS

Instrumental techniques
• More selective and sensitive
than volumetric & gravimetric.
• Instrumentation must be
calibrate.
• Calibration is accomplished by
preparing a series of standard
solutions of the analyte at
known concentrations.
• Calibration curve – instrument
response (function of
concentration).
 CALCULATING THE RESULTS
STEP 7
AND REPORTING THE DATA

 Calculate & Evaluate the results

 To estimate whether results are reliable or not:

1. PRECISION :estimate using the standard deviation

( based on replicate measurements)

2. ACCURACY :evaluate by refer to standard materials

Precision and accuracy is very important in analytical

chemistry and referred as quality control or quality
assurance
2. MOLES, MOLARITY, CONCENTRATION

UNITS FOR QUANTITY & CONCENTRATIONS

 Mole and milimoles

 Concentrations & its Definition
 Density and Specific Gravity
 Molarity, Molality
 Percentage Concentration:
 % w/w, % w/v, % v/v
 ppm, ppb, ppt
2. MOLES, MOLARITY, CONCENTRATION
UNITS FOR QUANTITY & CONCENTRATIONS

MOLE

• The mole (mole) is the SI unit for the amount

of a chemical species.
• 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 C12
atoms.
• The mass in grams of 1 mole of a substance is
called its molar mass.
2. MOLES, MOLARITY, CONCENTRATION
RELATIONSHIP BETWEEN MOLE & NUMBER OF
ENTITIES
MOLE
 1 mole of atoms/molecules/ions of any element will
contain Avogadro’s number of atoms/molecules/ions or
6.022 x 1023 atoms/molecules/ions of that element.

For example:
 1 mol of Mg atom contain 6.022 x 1023 Mg atoms.
 1 mol of H2O molecule contain 6.022 x 1023 H2O
molecules.
 1 mol of Na+ ions contain 6.022 x 1023 Na+ ions
EXERCISES

Number of entities = number of moles x (6.022 x 1023)

1. Calculate the number of atoms in 1 mol of aluminium atoms.

(6.02 x 1023)
2. Calculate the number of atoms in 0.5 mol of aluminium atoms.
(3.02 x 1023)
3. If a container has 12.0 x 1023 atoms of magnesium, determine
number of moles of magnesium atoms.
(2.0 moles)
4. How many molecules of CO2 are found in 3.5 moles of CO2?
(2.1 x 1024)
5. How many Cl- ions are present in 0.25 moles of CaCl2?
(3.0 x 1023)
2. MOLES, MOLARITY, CONCENTRATION
UNITS FOR QUANTITY & CONCENTRATIONS

MOLE & MILIMOLE

1 g= 1000 mg
1 mol = 1000 mmol
1 L = 1000 mL
EXAMPLE
EXAMPLE
EXAMPLE
FORMULA
EXERCISES
RELATIONSHIP BETWEEN MOLE & NUMBER OF ENTITIES

1. Calculate the number of moles for 3.4 g of carbon atoms.

(0.28 moles)
2. Find the mass of 0.30 moles of CH4
(4.8 g)
2. Calculate no of moles of Cl- is present in 0.34 moles of CaCl2
(0.68 moles)
4. Find the mass of H in 2.5 moles of H2O?
(5.0 g)
4. Find the mass of O in 3.0 moles of CO2?
(96.0 g)
2. MOLES, MOLARITY, CONCENTRATION

CONCENTRATION
WATER is considered a universal solvent for
most solutions

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.
2. MOLES, MOLARITY, CONCENTRATION

DENSITY & SPECIFIC GRAVITY OF SOLUTION

 Density of a substance is the mass per unit volume.

 In SI unit, density is expressed in unit of kg per liter, (kg/L) or in
metric system the unit use is gram per milliliter, (g/mL).
 Density of water = 1 g/ mL
 Specific gravity is the ratio of the mass of an equal volume
of water at 4oC.
 Specific gravity is dimensionless.
2. MOLES, MOLARITY, CONCENTRATION

MOLARITY OR MOLAR CONCENTRATION

 Molarity : no of moles of the solute in 1 L (dm3) of
solution
 Molar mass (atomic mass) - the mass of 1
mole of a substance in unit gram. (Unit for
molar mass is g/mol)
 Unit for Molarity (mol/L), (M), (mmol/mL)
M = no of mol of solute (mol)
volume of solution (L)
or
M = no of mmol of solute (mmol)
volume of solution (mL)
EXAMPLE

1. Calculate the molar concentration of ethanol in aqueous

solution that contains 2.30 g C2H5OH (46.07 g/mol) in 3.50 L
of solution

No of mole C2H5OH = 2.30 g = 0.04992 mol

46.07 g/mol

Molarity = 0.04992 mol = 0.0143 M

3.5 L
EXAMPLE
Try this!!
2. Sea water contains roughly 28.0 g of NaCl per liter.
What is the molarity of sodium chloride in sea water?

No of mole NaCl = 28.0 g = 0.4791 mol

58.44 g/mol

Molarity = 0.4791 mol = 0.4791 M

1L
EXAMPLE
3. What is the molarity of 5.30 g of Na2CO3 dissolved in
400.0 mL solution?

No of mole Na2CO3 = 5.30 g = 0.05 mol

106 g/mol

Molarity = 0.05 mol = 0.125

0.4 L
= 0.125

Remember!! 1 L = 1000 mL
• convert volume 1 dm3 = 1000 cm3
to L or dm3
2. MOLES, MOLARITY, CONCENTRATION

MOLALITY
 Number of moles of solute that dissolved in 1000 g of
solvent, m
 Preferred expression of concentration involving
colligative properties such as (boiling point
elevation, freezing point depression, osmotic
pressure)
 Unit for molality, m = (mol/kg)

FORMULA!!
m = no of mol of solute (mol)
1 kg of solvent (kg)
EXAMPLE
◦ 1. 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.

◦ Mol of Br2 = 10 g = 0.063 moles Br2

◦ (159.8 g/mol)

◦ Next, convert the volume of solvent to the weight of solvent using the
density
◦ = 1.00 L x 0.779 kg/L = 0.779 kg

◦ Now just divide the two to get the molality

◦ Molality, m = 0.063 moles Br2 = 0.080 molal
0.779 kg cyclohexane
EXAMPLE
Try this!!
2. A sulfuric acid solution containing 571.4 g of H2SO4 per liter of
solution has a density of 1.329 g/cm3. Calculate the molality of
H2SO4 in this solution

No of mol H2SO4 = 571.4 g = 5.826 mol

(98.0768 g/mol)

Mass of solvent:
1 L of solution = 1000 mL = 1000 cm3
1.329 g/cm3 times 1000 cm3 = 1329 g (the mass of the entire
solution)
1329 g - 571.4 g = 757.6 g = 0.7576 kg (the mass of water in the
solution)

Molality, m = 5.826 mol / 0.7576 kg = 7.690 m

3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

% CONCENTRATION

 Concentration can be described in term of % (percentage)

concentrations.

 % concentrations →% w/w
→% w/v
→% v/v
 Number of parts in 100 parts
 eg. Gram of A in 100 grams of sample.

% of A = number of parts of A x 100 %

number of parts of sample
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

1. % WEIGHT/WEIGHT TO EXPRESS THE

CONCENTRATION OF
% (w/w) COMMERCIAL REAGENTS

 Percent weight in weight concentration which is weight in 100 g

of sample.

 Weight percent (w/w) = weight of solute (g) x 100 %

weight of sample (g)

 Example: A nitric acid, HNO3 is sold as 70% solution.

-It means that the reagent contains 70 g pure per 100 g solution.

 70 % w/w = 70 g pure HNO3 x 100 %

100 g solution
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

1. % WEIGHT/WEIGHT
% (w/w) EXAMPLE
Calculate the molarity of the following acids

a) 70 % (w/w) HClO4, density = 1.67 g/mL

% d mm
70 g x 1.67 g x 1000 mL x 1.0 mol = 11.63 mol/L
100 g 1.0 mL 1.0 L 100.5 g

b) 96 % (w/w) H2SO4, density = 1.84 g/mL

% d mm
96 g x 1.84 g x 1000 mL x 1.0 mol = 18.02 mol/L
100 g 1.0 mL 1.0 L 98.0 g
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

1. % WEIGHT/WEIGHT
% (w/w) EXAMPLE
c) Briefly explain how to prepare the following solution in the laboratory. 500 mL
of 2.0 M H2SO4 from a commercial reagent at 90 % (w/w) purity and specific
gravity of 1.84.

90 g x 1.84 g x 1000 mL x 1.0 mol = 16.9 mol/L

100 g 1.0 mL 1.0 L 98.0 g

Molarity H2SO4 = 16.9 M,

Find volume need to transfer from commercial reagent H2SO4

McVc = MdVd , Vc = 2.0 M (500 mL) = 59.2 mL

16.9 M

So, measure and transfer 59.2 mL from commercial reagent to 500 mL of

volumetric flask. Dilute with distilled water until calibration mark. Shake upside
down.
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)
2. % WEIGHT/VOLUME TO INDICATE THE
COMPOSITION OF DILUTE
% (w/v) AQUEOUS SOLUTION OF
SOLID REAGENTS

 Percent weight in volume concentration which is weight in

100 mL of sample.
 Weight percent (w/v) = weight of solute (g) x 100 %
volume of sample (mL)

 Example: A 5 % aqueous silver nitrate refers, AgNO3 to

solution prepared by dissolving 5 g of AgNO3 in sufficient
water to give 100 mL of solution.

 5 % w/v = 5 g AgNO3 x 100 %

100 mL solution
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

2. % WEIGHT/VOLUME
% (w/v)
EXAMPLE
1. Briefly explain how to prepare the following solutions ( 1.0 L, 10.50 % (w/v)
aqueous CH3CH2CH2OH

% (w/v) = mass (g) x 100 , 10.5 % = mass (g) x 100,

volume (mL) 1000 mL

So mass CH3CH2CH2OH = 10.5 (1000 mL) = 105 g

100

Weight 105 g of CH3CH2CH2OH, dissolve with small amount of distilled water, transfer to
1.0 L of volumetric flask, dilute with distilled water to the calibration mark. Shake upside
down.
3. EXPRESSION OF CONCENTRATION (PERCENTAGES %)

3. % VOLUME/VOLUME TO SPECIFY THE CONCENTRATION

OF A SOLUTION PREPARED BY
% (v/v) DILUTING A PURE LIQUID WITH
ANOTHER LIQUID

 Percent volume in volume concentration which is volume in

100 mL of sample.
 Weight percent (w/v) = volume of solute (mL) x 100 %
volume of sample (mL)

 Example : A 5 % aqueous methanol solution means 5 mL of

methanol dissolve in enough distilled water to make 100 mL
solution.

 5 % v/v = 5 mL ethanol x 100 %

100 mL solution
3. ANOTHER EXPRESSION OF CONCENTRATION

4. ppt, ppm, ppb

(for SOLID & LIQUID)
 Part per thousand (ppt), part per million (ppm) and part per billion
(ppb)
 For sample that contain smaller amount of component the
concentration is expressed in terms of ppt, ppm or ppb.

1. ppt = parts per thousand (103) :

Number of parts of a substance found in one thousands parts
of a particular gas, liquid or solid.
2. ppm = parts per million (106) :
Number parts of a substance present in one million parts of
solvent (water)
3. ppb = parts per billion (109)
Number parts of a substance present in one billion parts of
solvent (water)
3. ANOTHER EXPRESSION OF CONCENTRATION

4. ppt, ppm, ppb

(for SOLID & LIQUID)

• ppb = parts per billion (109)

• pptr = part per trillion (1012)
• Eg : ppm(106)
If we use gram as the unit, 1 ppm means we have 1 g of substance
in 1,000,000 g solvent.
3. ANOTHER EXPRESSION OF CONCENTRATION

4. ppt, ppm, ppb

(for SOLID & LIQUID)
Expression (unit) of concentration ppt/ppm/ppb in terms of
percentage of w/w, w/v & v/v

w/w v/v w/v FACTOR

g/g x 103 mL/mL x 103 g/mL x 103
103
ppt mg/g mL/L mg/mL
g/kg µL/mL g/L
g/g x 106 mL/mL x 106 g/mL x 106
106
ppm mg/kg µL/L mg/L
µg/g nL/mL
g/g x 109 mL/mL x 109 g/mL x 109
ppb 109
µg/kg nL/L µg/L
3. ANOTHER EXPRESSION OF CONCENTRATION

4. ppt, ppm, ppb

(for SOLID & LIQUID)

EXAMPLE
1. What is the w/v in ppm of sodium in a solution containing 2.500mg of Na+
in 500 mL of solution.

ppm (w/v) = mg of analyte = 2.500 mg = 5 ppm

L of solution 0.5 L

Or

ppm (w/v) = g of analyte x 106

ml of solution
= 2.5 x 10-3g x 106
500mL
= 5 ppm
EXAMPLE
2. An analysis for cadmium in water give a value of
1.20 ppb (w/v). What mass of cadmium is
contained in 1.00 L water?
ppb = g/mL x 109

? g x 109 = 1.20
103 mL

?g = 1.2 x 103
109
= 1.2 x 10-6 g
= 1.2 µg
EXAMPLE
3. Determine the ppm of ferrous ion, Fe2+, in a solution known
to be 1.2 × 10-6 M Fe3(PO4)2.8H2O
(RMM=501.61)
EXAMPLE
4. Describe the preparation of 1L 0.1 M HCl from
concentration HCl 37% w/w and with density 1.18 g/mL
EXAMPLE
1.Molarity (concentrated) = percentage (%) x
(density/RMM) X 1000
2.M1V1 (concentrated) = M2V2 (diluted)
Using 2 formula:
EXAMPLE
EXAMPLE
5. Describe the preparation of a 250 mL 50 ppm solution
of AgNO3 from solid chemical.
EXAMPLE
6. Describe the preparation of 0.5 L 50 ppm of Cl- from
solid KCl.
EXAMPLE
7. How many gram of Ba(NO3)2 is needed to prepare a 50mL
solution containing 100 ppm NO3-?
EXAMPLE
EXAMPLE
EXAMPLE
EXAMPLE
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?
EXERCISES
1. Define:
a) Parts per million
b) Molality
c) Molarity
d) Percentage

2. Calculate the number of mole in the following: i) 250

ml, 0.150 M HCl (Ans: 0.0375 mole)
ii) 6.72 liter H2 at STP. (Ans: 0.3 mole)

Hint: 1 mol of H2 at STP contain 22.4 L

EXERCISES
3. How many mole of solute present in the
following solutions:
i) 16.3 liter solution 0.113 M (Ans: 1.8419 mole)
ii) 15.6 ml solution 0.025 M (Ans: 0.0039 mole)

4. Calculate the molar concentration of ethanol in an

aqueous solution that contains 2.30 g of C2H5OH (46
g/mol) in 3.5 L of solution
(Ans: 0.0143 M)

5. Calculate the molarity of 15.0 g ammonia in 750

mL solution. (Ans: 1.1765 M)

6. Briefly explain how to prepare the following solutions;

500 mL 6.50 % (w/v) aqueous ethanol, C2H5OH.