BITS Pilani

K K Birla Goa Campus

EE ZG514/ SSTM ZG516: Environmental Sampling

and analytical methods
Dr. Sharad M. Sontakke
Lecture - 1 Department of Chemical Engineering
BITS Pilani, K K Birla Goa Campus
Why Environmental Analysis (EA)?
To monitor and study levels of pollutants in the environment
To ensure the quality of air/water/soil with the regulatory
guidelines
To decide implementation of the control measures

Example:
1. Analysis of surface and ground waters prior to their use
for drinking water.
2. Air quality analysis to monitor the emission levels of
harmful gases

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Sampling: Method of collecting representative material for
analyzing the properties of interest

Objectives:
To provide preliminary information about the site or material
being analyzed (Exploratory sampling)
To provide information on the variation of specific analyte
(components of a sample) concentration over a period of
time or within a specific geographical area (Monitoring)

Example: Sampling from an industrial site which is suspected

to pollute a nearby river, sampling of water from a river
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Contents

1. Course overview
2. Textbooks/ reference books
3. Evaluation scheme
4. Module 1 (part 1): Structure and function of pollutants,
and analysis
• Structural formula
• Functional groups
• Organic pollutants
• Inorganic pollutants

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Course overview
Error analysis,
Nature of Mass
Standardization and
pollutant spectrometry
calibration

Environmental Sampling
and Analytical methods

Separation
methods Electrochemical Spectrochemical
HPLC, GC, LC- Analysis Analysis
MS Chemical UV-Vis, Fluorescence,
Equilibrium, IR, AAS, etc
Potentiometer
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Questions that need to be addressed:

1. How much sample do we need for analysis?

2. How do we ensure it is an representative sample?

3. How to select an appropriate analytical technique?

4. How to account for errors during the calculation?

5. How to convey the results in acceptable format?

6. How each of the analytical method works?

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Textbooks/ reference books

T1: Fundamentals of Analytical Chemistry, Douglas A. Skoog,

Donald M. West, F. James Holler, Stanley R. Crouch, 9th
Edition, Cengage Learning
T2: Introduction to Spectroscopy, Donald L. Pavia, Gary M.
Lampman, George S. Kriz, James R. Vyvyan, 4th Edition,
Cengage Learning
T3: Principles of Environmental Chemistry, Second Edition,
James E. Girard, Jones & Bartlett Learning
R1: Research papers
R2: Analytical Chemistry, Gary D. Christian, Sixth Edition

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Evaluation Scheme

As per the time-table

As per the time-table

Syllabus for Mid-Semester Test: will be announced

Syllabus for Comprehensive Exam: All topics (Lecture 1 to final lecture)

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Module 1 (part 1): Structure and function of
pollutants, and analysis

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Introduction

Pollutants in water:
Ions, heavy metals, chemicals
(causing color, odor,
unacceptable taste, health
hazard), agrochemicals,
microorganisms, dissolved
solids, radioactive elements, Carbon monoxide (CO),
etc. sulfur dioxide (SO2), nitrogen
oxides (NOx), volatile organic
compounds (VOCs; mostly
hydrocarbons [HCs]) and
suspended particles are the
five primary air pollutants
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Type of analysis

Qualitative analysis reveals the identity of the elements and

compounds in a sample.
A qualitative analysis is often an integral part of the
separation step, and determining the identity of the
analytes.

Quantitative analysis indicates the amount of each

substance in a sample.
Example: Quantities of hydrocarbons, nitrogen oxides,
and carbon monoxide present in automobile exhaust gases
are measured to determine the effectiveness of emission-
control devices.

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Sampling

An analysis must be performed on a sample that has the

same composition as the bulk of material from which it
was taken in order to produce meaningful information.

Sampling is the process of collecting a small mass of a

material whose composition accurately represents the
bulk of the material being sampled.

Sampling is frequently the most difficult step in an analysis

and the source of greatest error.

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Analytic methods

Some examples:
• UV-Vis spectroscopy
• Fourier transform infra-red spectrometry (FTIR)
• Gas chromatography (GC)
• Mass spectroscopy (MS)
• Liquid chromatography (LC)
• Atomic absorption spectroscopy (AAS)
• Potentiometry, etc.

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Structural formula

Sucrose (common sugar): C12H22O11

Ethyl alcohol: C2H5OH
Methane: CH4

Molecular formula: Atoms of each elements present in the

compound
Structural formula: Describes the bonding between the
elements

Sucrose Ethyl alcohol Methane

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Structural formula

Hydrocarbons (HCs):
HCs are the organic chemicals that are solely made up of C
and H.

C-C single
bond
(saturated) C-C double/
triple bond
Ring structure with
(unsaturated)
delocalized pi-
electrons
Source: https://www.britannica.com/science/hydrocarbon/Cycloalkanes accessed on 7th Jan 2021
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Alkanes (CnH2n+2)

Different compounds that

have the same molecular
formula are called
isomers

Isomers can have

different physical and
Straight chain Branched chemical properties
Source: https://www.britannica.com/science/hydrocarbon/Cycloalkanes accessed on 7th Jan 2021
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Cycloalkanes (CnH2n)
Saturated hydrocarbons with presence of cyclic structure, having two
hydrogen atoms less than an alkane.

Alkenes (Olefins, CnH2n) and alkynes (CnH2n-2)

Unsaturated hydrocarbons

Source: https://www.britannica.com/science/hydrocarbon/Cycloalkanes accessed on 7th Jan 2021

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Aromatic hydrocarbons

Benzenoid aromatic compounds: Containing benzene ring

Non-benzenoid aromatic compounds: aromatics which lack benzene ring

Mono-substituted derivatives of
benzene

Source: https://www.britannica.com/science/hydrocarbon/Cycloalkanes accessed on 7th Jan 2021

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Alcohols:
Organic compounds that that contain one or more hydroxyl (-
OH) groups attached to a single bonded alkane

Ethanol (ethyl alcohol)

Phenols: Phenols are compounds consisting of a hydroxyl

group (OH) and an aromatic carbon ring

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Functional groups

Functional groups are groups of atoms within a molecule that

confer specific chemical properties to the molecules.

Source: https://bio.libretexts.org/Courses/University_of_California_Davis/BIS_2A%3A_Introductory_Biology_-
_Molecules_to_Cell/MASTER_RESOURCES/Functional_Groups accessed on 7th Jan 2021

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Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021

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Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021

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 Example: drug molecule morphine

multifunctional

Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021

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Properties of alcohols

Alcohols are polar compounds

In relation to alkanes of comparable size and molecular
weight.
They have higher boiling points
They are more soluble in water
The presence of additional -OH groups in a molecule
further increases solubility in water and boiling point

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Properties of carboxylic acid

Carboxylic acids have significantly higher boiling points than

other types of organic compounds of comparable molecular
weight
They are polar compounds and form very strong
intermolecular hydrogen bonds
Carboxylic acids are more soluble in water than alcohols,
ethers, aldehydes, and ketones of comparable molecular
weight
They form hydrogen bonds with water molecules through their
C=O and OH groups

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Concentration Units

Molarity and Molar Solutions

For aqueous solutions, the unit of concentration that is most
often used by chemists is molarity—the number of moles
of solute per liter of solution.

Seawater, for instance, contains 1.06% of Na+ (percentage

weight/volume, or weight of Na per 100 mL of solution).
Thus, to convert 1.06% Na+ to molarity of Na+, do the
following. First, determine how many grams of Na+ would
be present in 1 L of seawater:
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Thus, in 1 L:

Now determine how many moles are present in 10.6 g of

Na+:

Thus seawater has a molarity (M) of Na+ of 0.46 M.

(Note: gmole is defined as weight in g/ Mol. Wt.)

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For elements or chemicals that are present at low
concentrations, it is often more convenient to express the
concentration in millimolar (millimoles, [10–3]/L), micromolar
(micromoles, [10–6]/L), or nanomolar (nanomoles, [10–9]/L)
units.

Parts per Million

The unit ppm is a convenient way to describe very dilute
solutions. It is frequently used for stating concentrations of
pollutants in water.
Consider drinking water in which the concentration of
dissolved lead is 1 ppm. This means there is 1 part lead in
every 1 million parts water.
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Parts can be expressed in any unit of mass (e.g., ounces,
tons, micrograms), but the same unit must be used for
both solute and solvent. We use grams:

Because it is more convenient to measure liquids by volume

rather than by mass, we change the mass of water to a
volume of water: 1 g of pure water has a volume of 1 mL
(density = 1.00 g/mL). Therefore,

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We change milliliters to liters:

We change grams to milligrams:

Therefore: 1 ppm = 1 mg/L

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Determine how many moles of solute are present in the
solution that contains 1 ppm lead?

To convert to moles, divide 1 mg by lead’s gram molecular

weight:

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Parts per Billion
For certain solutions - particularly water samples containing
minute traces of contaminants- it is often more convenient
to express concentration in ppb rather than ppm.

1 ppb = 1 µg/L

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Exercise

The U.S. EPA set a limit for the concentration of lead in

drinking water at 15 ppb. A laboratory finds the
concentration of lead in a sample taken from a water
fountain to be 18 µg/100 mL. Is this above or below the
EPA limit? By how much?

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Organic pollutants

These includes organic compounds such as:

• Phenols,
• Organic dyes,
• Polyaromatic hydrocarbons,
• Polychlorinated biphenyls,
• Pesticides,
• Pharmaceuticals,
• Polymers, etc.

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Inorganic pollutants

These include:
• Heavy metals and trace elements such cadmium
(Cd), chromium (Cr), arsenic (As), lead (Pb), mercury
(Hg), Fluoride (F), etc.,
• Oxides of metal,
• Inorganic ions: Chloride (Cl‒), Sulfate (SO42‒),
(NO3‒), Phosphate (PO32‒), etc.
• Metal salts, etc.

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Summary

In this lecture we have discussed:

• Need of environmental sampling and analysis
• Qualitative and quantitative analysis
• Structural formula
• Functional group
• Concentration unit
• Organic and inorganic pollutants

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Questions
1. What are the objectives of Environmental analysis?
2. What is the difference between qualitative and quantitative
analysis?
3. What is sampling?
4. How a structural formula is different from molecular
formula?
5. What is the difference between saturated and unsaturated
hydrocarbons?
6. What are the functional groups for alcohols and phenols?
7. What is the functional groups for carboxylic acids?
8. Are pesticides example of organic pollutants?
9. Are heavy metals example of organic pollutants?
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Plan for next lecture

• Sources of organic/inorganic pollutants

• Common analytical methods
• Sampling methods

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