CHAPTER 4

ENVIRONMENTAL
SAMPLING AND
ANALYSIS
 4.1 Introduction
• Sample is a portion of a system (environment),
representative for the sampling place and moment.
• Environmental sampling is about observing the traits of a
specified environment.
• There are many different sampling methods – how you
choose to sample your environment will depend on the
nature of your habitat and study species.
• Samples are complex homogenous systems (solutions) or
heterogeneous ones.
• Rarely we analyze a mono-component sample, in most of
the cases, the real samples are multicomponent systems,
consisting in compounds that are present as major
component, or as trace components.
 Cont.…
• There are several areas for which sampling and environmental
analyses are required:
1. Routine Monitoring – for example to measure concentration of
pollutants in the environment and to identify short- and long-
term trends;
2. Emergency Response – for example to detect accidental
release of pollutants in the environment and to evaluate risk and
toxicity of humans and biota;
3. Regulatory Enforcement And Regulatory Compliance –to
measure how much pollutants are released into environment in
order to comply with regulatory requirements;
4. Scientific Research –to study the fate and transport of
contaminants and evaluate the efficiency of remediation systems.
4.2 Typical compounds present in air, water and soil
Cont.…
• Sampling is the generic term consisting in two
distinguished groups of operations:
• Pre Laboratory Operations – consisting in
(i) on-site sample up-take/collection (usually also
called “sampling”),
(ii) on-site conservation,
(iii) transportation and storage;
• In Laboratory Operations – consisting in sample pre-
treatment and preparation for analysis; these include
separation, purification, concentration, or other
operations.
 Cont.…
• For the compounds that could suffer considerable transformations
during the transport to the laboratory, samples should be
analyzed on-site.
 4.3 Environmental Samples Preservation And Storage
• are pre-laboratory stages, aiming to avoid physical or chemical
processes that might occur during the transportation of the samples
to the laboratory.
• Physical processes such as volatilization, diffusion, absorption are
avoided by cooling and by choosing the appropriate sampling and
storage containers.
• Chemical, biochemical processes, as well as microbial degradation,
are also avoided by cooling and choosing the appropriate recipients,
additionally by adding chemical reagents, so-called preservatives.
• preservatives may react with certain compounds in the sample,
which is accepted practiced as long as the chemical reaction is
complete, qualitatively and quantitatively controlled.
• These chemical processes will be taken into account during the
calculations that will lead to express the final result
Cont.…
• Figure blow are presented several samples collected
for environmental analysis, stored in different
containers, like plastic flasks or bags.
Environmental samples preservation
Sample Pre-treatment / Preparation

• Sample pre-treatment / preparation is the second group of

operations, as pre-analysis stage, to be performed on the
samples, in the laboratory.
• The purpose of sample preparation is to bring the samples in
a measurable form. Sample preparation involves operations
aiming both the sample and the analyze:
Separation method used in the sample pre-treatment
Most of the operations used in sample pre-treatment are
based on separation processes and there are several
modes to classify and group them.
The classification is based on different phase equilibrium:
1. Gas–liquid Equilibrium: absorption, extraction,
distillation;
2. Gas–solid Equilibrium: adsorption, extraction;
3. liquid–liquid equilibrium: liquid-liquid extraction
techniques;
4. liquid–solid equilibrium: filtration, centrifugation,
ad/absorption, solid phase extraction (solid phase micro
extraction, solvent extraction)
 4.4 Environmental Analysis
• An environmental analysis is a strategic technique used
to identify all internal and external factors that could
affect an environment.
• Analytical chemistry is the science that studies and uses
methods and instruments developed to separate, identify,
and quantify the composition of matter/sample.
• Chemical analysis represents a sum of on-site or in-lab
operations performed to give qualitative and quantitative
information about the composition of a complex sample.
• Chemical analysis of a sample consists in characterizing it
from the point of view of its chemical composition and, in
principle, is based on a measurable property of the solute
(analyte), sometimes of the solution (sample).
 Analytical Methods Principles
• Analytical methods principles are based on a measurable
property (P) of the analyte (A): mass, volume, thermal,
electrical, or optical property.
• The determination of the chemical composition of a
sample imposes two types of information to be acquired:
qualitative information (qualitative analysis, or
identification); quantitative information (quantitative
analysis, or quantification).
• Quantitative analysis means to find the measurable
property (P) that can be related as a function of the
analyte concentration (CA), based on physical chemical
laws: P=f(CA).
 Classification Of The Environmental Analytical Methods
• Analytical methods can be grouped into two categories:
1. Classical Analytical Methods – also called wet chemical
methods; were firstly developed, being dependent on technology
development in time, and are based on chemical reactions that
occur between the analyte and specific reagents, therefore they are
destructive methods.
2. Modern Or Instrumental Analytical Methods; analytes are
subject of physical transformation during the measurements, thus
being non-destructive methods; these methods use calibration
curves for quantitative determinations obtained on standard
solutions. They are more recently developed, based on physical
transformation of the analyte, therefore are non-destructive.
Table Methods and techniques used for environmental analysis
 4.5 Method Validation
• It is the process of defining an analytical requirement, and
confirming that the method under consideration has
performance capabilities consistent with what the
application requires.
• Validation is also considered to give the confirmation by
examination and provision of objective evidence that the
particular requirements of a specified intended use are
fulfilled, or fit to purpose.
• To validate a method is compulsory to demonstrate the
following method performance criteria: specificity /
selectivity, precision, trueness, linearity and linearity
range, limit of detection (LOD), limit of quantification
(LOQ), and ruggedness / robustness.
Cont.…

• A method should be validated whenever a change in the

analytical process occurs, and the laboratory has to
demonstrate that its performance parameters are adequate
for its use for a particular analytical problem, meaning:
• new method was developed;
• the existing method was revised;
• method is changing with time;
• method is used in a different laboratory, or with
different analysts or different instrumentation;
• the method is equivalent with another one, for
example a standard one.
 4.5 Uncertainty Estimation
• uncertainty (U) is a parameter associated with the result of a
measurement, that characterizes the dispersion of the values
that could reasonably be attributed to the measured (result).
• Uncertainty may be expressed as relative standard deviation
(RSD) and confidence interval.
• Uncertainty estimation is required whenever:
• a new procedure/method is introduced in the laboratory;
• an important process parameter is modified (equipment,
sample type);
• a new method is validated;
• not required for daily analysis.
Cont…

• There are two steps to follow in order to estimate

the uncertainty:
1. identifying the uncertainty sources and build up
the Ishikawa diagram;;
2. uncertainty calculation, considering the
sources, that have the most relevant contribution
to the total uncertainty.
4.6 Noise Pollution And Control
• Noise pollution is, unwanted or excessive sound that
can have Deleterious effects on human health,
wildlife, and environmental quality.
• Noise pollution is commonly generated inside many
industrial facilities and some other workplaces, but it
also comes from highway, railway, and airplane traffic
and from outdoor construction activities.
 Measuring and perceiving loudness
• Sound waves are vibrations of air molecules carried from
a noise source to the ear.
• Sound is typically described in terms of the loudness (
amplitude) and the pitch (frequency) of the wave.
• Loudness (also called sound pressure level, or SPL) is
measured in logarithmic units called decibels (dB).
• The normal human ear can detect sounds that range
between 0 dB (hearing threshold) and about 140 dB, with
sounds between 120dB and 140 dB causing pain (pain
threshold).
 Cont…
• Precise measurement and scientific description of sound levels
differ from most subjective human perceptions and opinions
about sound. Subjective human responses to noise depend on
both pitch and loudness. Sound below or above 80db is
considered to be sound pollution.
• The so-called A-weighted filter, for example, is commonly used
for measuring ambient community noise.
• SPL measurements made with this filter are expressed as A-
weighted decibels, or dBA.
• Most people perceive and describe a 6- to 10-dBA increase in an
SPL reading to be a doubling of “loudness.”
• Another system, the C-weighted (dBC) scale, is sometimes used
for impact noise levels, such as gunfire, and tends to be more
accurate than dBA for the perceived loudness of sounds with low
frequency components.
Effects on humans and wildlife

• At certain levels and durations of exposure, it can cause physical

damage to the eardrum and the sensitive hair cells of the
inner ear and result in temporary or permanent hearing loss,
known as noise-induced hearing loss.
• Hearing loss does not usually occur at SPLs below 80 dBA (eight-
hour exposure levels are best kept below 85 dBA), but most
people repeatedly exposed to more than 105 dBA will have
permanent hearing loss to some extent.
Cont….

• In addition to causing hearing loss, excessive noise

exposure can raise blood pressure and pulse rates,
cause irritability, anxiety, and mental fatigue, and
interfere with sleep, recreation, and personal
communication.
• Children living in areas with high levels of noise
pollution may suffer from stress and other problems,
such as impairments in memory and attention span.
• Noise pollution control is therefore important in the
workplace and in the community.
 Cont…
• Noise pollution also impacts wildlife. A wide range of animals,
including insects, frogs, birds, and bats, rely on sound for a
variety of reasons.
• Noise pollution can interfere with an animal’s ability to attract a
mate, communicate, navigate, find food, or avoid predators and
thus can even be an existential threat to vulnerable organisms.
• much of the world’s oceans are polluted with chaotic sounds
from ships, seismic tests, and oil drills.
• Some of the loudest and most detrimental sounds in the sea are
from naval sonar devices, whose noise can travel hundreds of
miles through the water and is associated with mass stranding's
of whales and dolphins.
Noise regulation and mitigation

• Noise-control ordinances and laws enacted at the local,

regional, and national levels can be effective in
mitigating the adverse effects of noise pollution.
• Example, Environmental and industrial noise is
regulated in the United States under the Occupational
Safety and Health Act of 1970 and the Noise Control
Act of 1972.
• Under these acts, the
Occupational Safety and Health Administration set up
industrial noise criteria in order to provide limits on the
intensity of sound exposure and on the time duration
for which that intensity may be allowed.
Cont…