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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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?
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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)
BITS Pilani, K K Birla Goa Campus
Module 1 (part 1): Structure and function of
pollutants, and analysis
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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.
BITS Pilani, K K Birla Goa Campus
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.
BITS Pilani, K K Birla Goa Campus
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.
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021
BITS Pilani, K K Birla Goa Campus
Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021
BITS Pilani, K K Birla Goa Campus
Example: drug molecule morphine
multifunctional
Source: https://www.chem.fsu.edu/chemlab/chm1046course/functional.html accessed on 7th Jan 2021
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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:
BITS Pilani, K K Birla Goa Campus
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.)
BITS Pilani, K K Birla Goa Campus
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.
BITS Pilani, K K Birla Goa Campus
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,
BITS Pilani, K K Birla Goa Campus
We change milliliters to liters:
We change grams to milligrams:
Therefore: 1 ppm = 1 mg/L
BITS Pilani, K K Birla Goa Campus
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:
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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?
BITS Pilani, K K Birla Goa Campus
Organic pollutants
These includes organic compounds such as:
• Phenols,
• Organic dyes,
• Polyaromatic hydrocarbons,
• Polychlorinated biphenyls,
• Pesticides,
• Pharmaceuticals,
• Polymers, etc.
BITS Pilani, K K Birla Goa Campus
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.
BITS Pilani, K K Birla Goa Campus
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
BITS Pilani, K K Birla Goa Campus
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?
BITS Pilani, K K Birla Goa Campus
Plan for next lecture
• Sources of organic/inorganic pollutants
• Common analytical methods
• Sampling methods
BITS Pilani, K K Birla Goa Campus