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CHAPTER 1

INTRODUCTION: ANALYTICAL
CHEMISTRY

SITI MAZLEENA
MOHAMED
SMM/FSG/UiTM NS

CHAPTER OUTLINE

Review the type and steps in analysis


Review the terms: Moles, molarity and
concentration.
Review other forms of expressing concentration
i) ppm
ii) ppb
iii) ppt
iv) %(w/w)
v) %(w/v)
vi) %(v/v)
SMM/FSG/UiTM NS

What is chemical
analysis?

A field that related to the measurements and


characterization of a chemical species that contain in a
sample

Chemical analysis is more than just detecting or


determining the general composition or a specific
component of a sample.

It is the resolution or interpretation of a given problem.

SMM/FSG/UiTM NS

Discipline of analytical
chemistry
Qualitative
To detect the presence of a
substance in the sample

Quantitative
Is the determination of that
substances

Finding out what substances Finding the amount


(quantity) of substances

SMM/FSG/UiTM NS

Steps in analysis
Defining the problem
Selecting the method
Obtain a representative sample
Prepare the sample for analysis
Performing the measurements
Conducting the experiment and gathering the
data
SMM/FSG/UiTM NS

1. Defining Problem

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

Should know the origin of the sample.

Sample history include information on how, where, and


when the sample were collected, transported and stored.

Analyst will use the sample history to maximize


advantage in solving the problem.

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

3. Obtain a representative sample

Sampling: Process of selecting representative material


from the lot and storing the sample. (Define the term
sampling Apr 2007, Oct 2007)

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.

Continue

Homogeneous: Substance that


composition throughout the sample.

has

the

same

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.

4. Prepare the sample for analysis


Step of sample preparation involved bulk materials:
(Describe the steps involved in sampling bulk materials
Apr 2007)

1.

2.

Bulk sample must be reduced in size to obtain a


laboratory sample of several grams from which a few
grams to milligrams will be taken to be analyzed
(analysis sample).

The size reduction may require taking portions (eg,


two quarters) and mixing, in several steps, as well
as crushing and sieving to obtain a uniform
powder for analysis.

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:
i) reduce and remove interferences
ii) adjust analyte concentrations to a range suitable
for measurement
iii) produce species from analyte that have
quantitatively measurable properties.

5. Performing the measurements

Analysis: Incorporates the measurement of the


concentration of the analyte in replicates and comparing
with standards.

Replicate measurement: the practice of taking multiple


readings. (What do you understand by the term replicate
Nov 2005)

The replicate measurements are necessary to obtain the


measurement uncertainty.

The uncertainty important as it indicates the reliability of


the measurements.

6. Conducting the experiments

Factors:
i)
ii)

Calibration

Validation/Controls/Blank A blank contains the


reagents and solvents use in analysis, but no
analyte.

7. Gathering the result & report the data

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.

In class revision (1)


1.Calculate the molar mass of
formaldehyde?

2.Calculate the number of grams in one


mole of CaSO4. 7H2O

3.Calculate the molar mass of glucose?

SMM/FSG/UiTM NS

Moles

Moles =

grams
formula weight (g/mol)

Milimoles =
miligrams
Formula weight (mg/mmol)

SMM/FSG/UiTM NS

Homework (1)
1.

2.

How many moles and milimoles of


benzoic acid (molar mass = 122.1
g/mol) are contained in 2.00 g of the
pure acid?
How many grams of Na+ (23.00 g/mol)
are contained in 25.0 g of Na2SO4 (142
g/mol)?

SMM/FSG/UiTM NS

3. Calculate the number of the moles in


500 mg Na2WO4 (Sodium Tungstarte)

4. How many milligrams are in a 0.250


mmol Fe2O3 (ferric oxide)

SMM/FSG/UiTM NS

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

1 g = 1000 mg

formula weight
=

500 mg/1000
293.8

= 0.0017 mol

SMM/FSG/UiTM NS

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
SMM/FSG/UiTM NS

How do we express
concentrations of
solution?

Molarity (M) : No of moles of the solute in 1L


of solution.
M = no.mol solute
no.L solution

Milimoles = molarity x mililiters

Molality (m) : No of moles of the substance


per kilograms of the solvent.
m = no.mol solute
kg solution
SMM/FSG/UiTM NS

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

SMM/FSG/UiTM NS

Try this
How many grams Na2SO4 should be weighted
out to prepare 500 mL of a 0.100 M solution?

Ans: 7.1 g
SMM/FSG/UiTM NS

Density Calculations How do


we convert to molarity?
The
concentration
of
many
fairly
concentrated commercial acids and bases
are usually given in terms of percent by
weight.
It is necessary to prepare solutions of a
given approximate molarity from these
substances
Must know the density in order to calculate
molarity
SMM/FSG/UiTM NS

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.
SMM/FSG/UiTM NS

Continue

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.
Solution:
1)Formula weight of KOH = 39 + 16 + 1 = 56 g/mole.
2)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 = SMM/FSG/UiTM
1280 g. NS

Continue

3) 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 = 320 g
100
4) 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
SMM/FSG/UiTM NS
56 (g/mole)

Exampl
e:

How many milliliters of concentrated sulfuric acid, 94.0%


(g/100 g solution), density 1.831 g/cm 3, are required to
prepare 1 L of 0.100 M solution?

SMM/FSG/UiTM NS

Answer: 5.71 mL

Dilutio
n

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
SMM/FSG/UiTM NS

Example: To prepare 0.100 M HCl


solution

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:
Dilute 4.13 mL of concentrated acid in a 500-mL VF
Dilute with distilled water to the 500-mL mark
Invert the flask several times to ensure complete mixing.

1.
2.
3.

SMM/FSG/UiTM NS

Expressions of Analytical
Results
Solid sample

Weight percent, %w/w =

ppm = weight solute (g)

Weight solute (g)


x 100
Weight of sample (g)
x 106

ppb = weight solute (g)

x 109

ppt = weight solute (g)

x 1012

weight sample (g)

weight sample (g)

weight sample (g)

SMM/FSG/UiTM NS

Expressions of Analytical
Results
Liquid sample

%w/v =

Weight solute (g)


x 100
Volume of sample (mL)

ppm = weight solute (g)


volume of sample (mL)

x 10 6

ppb = weight solute (g)


volume of sample (mL)

x 10 9

ppt = weight solute (g)


volume of sample (mL)

x 10 12

SMM/FSG/UiTM NS

Common unit to express


content
Expression
Parts per
million

Parts per
billion

Abbreviation
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

SMM/FSG/UiTM NS

Example: Percent Composition

Briefly explain how to prepare 1.0 L 10.50% (w/v)


aqueous CH3CH2CH2OH

Solution:
%w/v = weight solute (g)
volume sample (mL)

x 100

10.50 = weight solute x 100 = 105 g


1000
SMM/FSG/UiTM NS

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

SMM/FSG/UiTM NS

Example: To prepare a solution of certain


molarity

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.

Solution:

1 M = 1000 mM

M = mol
L

M x V = 10.00 x 10-3 x 0.500 L = 5.000 x 10-3 mol


Weight of reagent = 5.000 x 10-3 mol x 249.69 g/mol
= 1.248 g
Procedure:
1. Place solid CuSO4.5H2O (1.248 g) into 500-mL volumetric flask.
2. Add some distilled water ~400-mL, stir to dissolve the solid reagent.
3. Add distilled water to the 500-mL mark.
4. Then, invert the flask several times (10x) to ensure complete mixing.
SMM/FSG/UiTM NS