Development

of a Sampling
Plan

1
 ▶ Samples c an inc lude ground
waters, surfac e waters,
drinking waters, industrial
effluents, hazardous wastes,
landfill leac hates, air
Environment emissions, soils, sediments,
vegetation, other biota.
al
▶ This great diversity makes
Samples sampling a challenge.
▶ All sample types should be
c onsidered when designing a
sampling plan for a specific
study.

2
 ▶ There are 4 main reasons
to collect and analyze
environmental samples:
Reasons for
Environment
▶ Survey
al Sampling
and Analysis ▶ Monitoring
▶ Regulatory
requirements
▶ Sc ientific study

3
 ▶ Survey obje ctives inc lude
the following:

Survey ▶ Establish baseline

environmental
Sample ▶
quality conditions.
Identify pollution
s sourc es.
▶ Assess long term
trends.
▶ Projec t future
c onditions.

4
 ▶ Monitoring objectives include
the following:

Monitorin ▶ Determine treatment

effic ienc ies for unit
g proc esses.
Predic t effec ts of
Samples ▶
disc harges.
▶ Determine health effe cts.
▶ Set water/soil/air
quality standards.

5
 ▶ Regulatory obje ctives inc lude
the following:

Regulator ▶ Verify self-monitoring data.

y ▶Verify c omplianc e with

permits.
Samples ▶ Support enforc ement ac tion.
▶ Support permit issuance or
re- issuance.

6
 ▶ Sc ientific study objec tives
inc lude the following:

▶ Produce effluents of
Scientifi ▶
the highest quality.
Optimize proc ess
c Study c ontrols.
▶ Determine the transport
and fate of pollutants in
the environment.
Samples ▶ Determine assimilative
capacities of air or
water bodies.

7
 ▶ In addition to the above,
spec ial programs may be set
up to assess the results of
environmental disasters.
▶ Such programs may
have obje ctives like:
▶ Survey the ba ckground to
determine what the normal
Environment level of pollution is.
al ▶ Monitor the specific disaster
Disasters area to determine the
additional pollution emitted.
▶ Produc e the information
needed to bring legal action
against the polluters and to
restore the environment to a
state of good health
(Occidental Chemical – NJ).

8
 9
Environmental disaster – A natural or
human- caused incident which results in a
negative or “disastrous” impact upon the
environment.

1. Fukushima Nuclear Plant – Japan

2. Gas Leak – Bhopal,

Environment India

al Disasters 3. C hernobyl Nuclear Power Plant –

Russia

4. Exxon Valdez Oil

Spill

5. Train Derailment – East Palestine,

Ohio
 1
Environmental 0
Disasters
▶ Case Summary: $165 Million Settlement to
Start Cleanup Work on the Passaic River in
New Jersey

▶ This settlement agreement will start the cleanup of the

largest environmental dredging project in the history of the
federal Superfund program. This is the first step in the
restoration of the Passaic River, which borders the
neighboring New Jersey communities of Newark, Harrison,
Kearny, Belleville, and Nutley.
▶ The cleanup work will remove 3.5 million cubic yards of toxic
sediment from the lower 8.3 miles of the Passaic, from
Newark Bay to the Newark/Belleville border.
 1
Environmental 1
Disasters
Did dioxins spread after the Ohio train
derailment?
After a catastrophic 38-train car derailment in East Palestine, Ohio, some
officials are raising concerns about a type of toxic substance that tends
to stay in the environment.
Concerns that exposure to the vinyl chloride itself could cause cancer
— may be more pressing than the possible dioxins.

Even so, most experts thought it was important to test the soils for dioxins
— even though that proc ess c an be diffic ult and c ostly.

The c onditions are right for dioxins to have been formed.

It's going to be terribly important to determine that from a public

health perspective, and to reassure the community.
 1
2

Environment
al Disasters –
Ohio Train
Derailment

Feb 3,
2023
 1
3

Environment
al Disasters –
Ohio Train
Derailment

Feb 3,
2023
 ▶ The objec tives of eac h study
affec t the design of the
sampling and analysis plan.
Sampling ▶ For survey work, there is
and flexibility in c hoosing the
number and location of samples
Analysis and analytical methods used.
Depends ▶ For example, suppose you
wanted to get an idea of the
on the general quality of drinking
water in C anada, but because
Objective of cost limitations, you c ould
look at only 6 different locations.
s Which ones would you
c hoose?

14
 ▶ In monitoring work, the
objec tives are usually more
Sampling ▶
c learly
For defined.
example, to see how
much SO2 is emitted from
and the top of a stac k it may be
Analysis nec essary to make
measurements every day for
Depends a year.
The stac k emissions may
on the ▶
c hange a lot between daytime
Objective and nighttime, so monitoring
may be needed twice a day.
s ▶ Continuous monitors may
be available.

15
 ▶ The most stringent sampling and
Sampling analysis schemes are needed
for regulatory ac tivities,
and be cause data may have to be
defended in a court of law.
Analysis ▶ The slightest deviation
Depends from standard protocols
may be enough to make
on the data indefensible.

Objective ▶ Without such data, it is impossible

to successfully prosecute
s polluters.

16
Sampling ▶ For researc h studies, the
sampling and analysis methods
and needed depend on the
spec ific objec tives of each
Analysis ▶
study.
Sometimes the nature of a
Depends researc h study requires
investigators to use methods
on the that are still experimental in
nature, and which may not give
Objective accurate results.

17
 ▶ There are many fac tors to
c onsider when developing a
sampling plan.
▶ The sampler should be aware of
these fac tors, but it’s seldom
nec essary to plan for all of
them in any single
investigation.
Factors in
▶ No matter how c omplete a
Environment sampling plan is, it’s always
al Sampling possible to encounter unexpected
situations.
▶ It’s important to keep in mind
the objec tives of the study
when planning and ca rrying
out the sampling.
▶ Some important fac tors to
c onsider when designing the
sampling plan are: 18
 ▶ Legal
c onsiderations;
▶ Will the results have to be
defended in a c ourt of law?
If so, a continuous chain of
custody of samples will have to
Factors in be shown from the time of
Environment sampling to analysis.
al Sampling
▶ Regulatory c onsiderations;
▶ Are the sampling and
analytic al methods to be used
specified by regulation?

19
2
0
 ▶ Types of samples
required.
▶ What kinds of samples must
be collected?
▶ Surfa ce water
▶ Ground water
▶ Drinking water
Factors in ▶ Industrial effluent
Environment ▶ Ambient air
al Sampling ▶ Precipitation
▶ Soil
▶ Sediment
▶ Hazardous waste
▶ Stac k emissions
▶ Biota

21
 ▶ Bac kground
samples;
▶ In addition to sampling
c ontaminated areas, samples
from outside the
c ontaminated area – not
thought to be c ontaminated
– are often needed.
▶ E.g., when trying to show that
Factors in c ontaminated effluent from an
industry is c ausing the river
Environment water downstream of the plant to
al Sampling be polluted, it is vital to also take
samples upstream of the plant –
to show the pollution was not
already in the river from some
other source.
▶ Suc h samples taken in non-
contaminated areas are
called background samples.

22
 ▶ Temporal
fac tors;
▶ Sometimes the time of the
year or even the time of day
affec ts pollution
measurements.

Factors in ▶ E.g., wood burning stoves

Environment and fireplac es may be
al Sampling used a lot in the winter, but
not in the summer.

▶ The way pollutants move in

the environment may be
different in the various
seasons bec ause of
temperature or other factors.

23
 ▶ Special pollution events suc h as
photoc hemic al smog depend
on the time of day and
atmospheric conditions.

▶ Industries may emit different

Factors in types or levels of pollutants
Environment depending on the time of year
or day.
al Sampling
▶ E.g., if a certain industrial process
c auses serious pollution
emissions from a smokestac k,
the industry may c hoose to
c arry out the proc esses at
night, so the sta ck emissions
are diffic ult to see.
24
 ▶ Spatial
fa ctors;
▶ Pollution gradients may exist in
air, water, or soil/sediment
samples.
▶ A water sample from the surfa ce
of a lake may c ontain a very
different level of pollution than
Factors in is found in water near the
Environment bottom of the lake.

al Sampling ▶ Soils c an have very different

levels of pollution in the top 1-2
c m c ompared to the levels at a
depth of 5-10 c m.
▶ The extent of suc h c oncentration
gradients depends on many
c omplex fac tors, inc luding the
physic a l and chemic a l
properties of the pollutant and
how the pollutant was released
to the environment. 25
 ▶ Ac c essibility of sampling
points;
▶ It is not always possible to take
a sample at the “ideal”
location.
▶ The sampling devic e may be
incompatible with the
Factors in specific area sampled, or it
may be too dangerous to
Environment approach the sampling
al Sampling point c losely.
▶ In such c ases, on-the-spot
dec isions must be made
to determine the best
possible sampling
loc ations.
▶ A complete written record must
be kept of such situations,
especially any observations
regarding the sampling 26
 ▶ Weather conditions;
▶ Air temperature, wind speed
and direction, and
precipitation are important to
rec ord during sampling.

Factors in ▶ Wind direction c an be

Environment c onfusing, because the
prevailing wind direction and
al Sampling speed may be different than
those observed directly at the
sampling site.

▶ These c onditions may also be

very different at ground level
c ompared to higher in the
atmosphere.
27
 ▶ Proximity of potential
pollution sources;

▶ What industries or other

Factors in possible sources of pollution
are c lose enough to affect
Environment the area sampled?
al Sampling
▶ E.g., automobiles from a major
highway will c ontribute
signific antly to the levels of
some pollutants

28
 ▶ Sample
contamination;
▶ Special c are must always be
taken to prevent sample
contamination.
▶ Some possible c auses of
sample contamination are:
Factors in ▶ Dirty sample containers
Sampling c ontainers made of
Environment ▶
the wrong material (e.g., glass
al Sampling versus plastic)
▶ Smoking during sampling
▶ Improper handling of sample
c ontainers (grease from
fingers, c ontamination from
gloves)
▶ Dust from the air
▶ Nearby industry
▶ Automobiles at a nearby
roadway 29
 ▶ Preservation of sample
integrity;
▶ The sample that is finally
analyzed is not always the
same as the sample that was
collected.
▶ E.g., some c ompounds in the
Factors in sample may react or
decompose to form different
Environment ones not originally present in
al Sampling the sample.
▶ Volatile c omponents will
eventually evaporate
from samples left sitting
too long.
▶ Steps must be taken to ensure
the sample that is analyzed is
representative of the one
originally c ollected (holding
times, proper c ontainers, 30
 ▶ Shipping and
storage;

▶ The way samples are

transported to the laboratory
and stored before analysis
and the length of time stored
Factors in are important considerations.
Environment
al Sampling ▶ E.g., most water samples must
be kept between 0 and 10°C
while being shipped.

▶ There are specified holding

times (the time from sampling
to analysis) for every kind of
analysis.

31
 ▶
Safety;
▶ Many unsafe field
c onditions can exist:
▶ Sampling near fast-
flowing streams
Factors in
Environment ▶ Sampling near
toxic c hemic al
al Sampling spills
▶ Sampling in
c onfined spaces
▶ In some c ases, spec ial
safety equipment is
required (i.e., moon suits,
Hazmat gear).
32
 ▶ Documentation;
▶ All sampling c onditions must
be recorded.

▶ Samples must be labelled so

they can be related to a
specific loc ation, date, and
Factors in time of sampling.
Environment
al Sampling ▶ The documentation should include
the name of the sampler.

▶ Proper doc umentation of unusual

c onditions that may affec t
results is especially important.

33
 ▶ Sub-Aliquoting;
▶ Samples taken in the field must often
be sent to several different analysts
to perform various determinations.
▶ E.g., it may be necessary to analyze a
soil sample for trac e metals, and for
organic c ontaminants suc h as PC Bs.
Factors in ▶ To do suc h different analyses on the
Environment same sample, it is necessary to
split the original sample into
al Sampling smaller portions (aliquots).
▶ Care must be taken so that the
aliquots are identic al to eac h other
and to the original.
▶ This may require special mixing or
grinding of the original sample whic h –
if not done properly – c an c hange the
results by analyte loss or sample
c ontamination.

34
 ▶ Filtration of aqueous
samples;
▶ Water samples usually
c ontain particulates.
▶ For many analytic al methods,
the particulate and aqueous
portions of the sample must be
separated and analyzed
Factors in individually (total vs. dissolved).

Environment ▶ However, the original sample

should be c ollec ted to make
al Sampling sure it c ontains the same
partic ulate distribution as
exists in the environment.
▶ It is easy to discriminate against
very small or very large
partic les.
▶ In some c ases, it may be
necessary to filter the
sample in the field.
35
 ▶ Filtration of aqueous
samples;

▶ Filtration c hanges the sample,

and if not done properly, c an
lead to incorrect results.
Factors in ▶ The analyte c oncentration in a
Environment filtered sample may be correct
but may not be the same as the
al Sampling c oncentration in the
environment.
▶ Filtering c an affect results by
introduc ing c ontamination, or
by analyte loss (the analyte
may stic k to partic ulates, glass
or other surfac es, or the filter).

36
 ▶ Quality
c ontrol;
▶ Elements of QC must be built
into every stage of sampling
and analysis.
▶ E.g., c ontainers must be pre-
c leaned before use. What
steps have been taken to
Factors in prove they really are c lean?

Environment ▶ Field blanks (FB) are taken to

the sampling site and treated
al Sampling exa ctly as the samples are –
exc ept that no a ctual sample
is added.
▶ If no analyte is found in the FB,
this is strong evidence that no
sample c ontamination has
taken pla ce.
▶ Field duplic ates may also be
taken to show if there is
imprec ision assoc iated with
sampling. 37
 ▶ C ost of
sampling;
▶ Sampling c an be quite expensive.

▶ Sometimes special equipment is

needed, that requires special training
to operate.
▶ Vehicles such as boats or airplanes
are sometimes needed.
Factors in ▶ It is always more costly to cut corners
Environment when sampling than to do it right the
first time.
al Sampling ▶ A hidden c ost of incorrect sampling
(hidden because the error may not be
detected) is that important decisions
may be made based on analytic al
results that are incorrect.
▶ E.g., citizens said that drinking water
is c ontaminated, but the samples
were c ontaminated only after they
were collected.

38
Sampling 3
9
Plan
▶ The overall sampling plan should consider all
the above factors.
▶ Some of the most important ones that
should always be considered are:
▶ Sampling loc ations
▶ Time of sampling
▶ Equipment needed
▶ Sampling containers (types, numbers, sizes)
▶ Types of samplers needed
▶ Logbooks
▶ C of C and other legal or regulatory needs
▶ Field QC proc edures
▶ Documentation needed including field observations to be
made
 ▶ The three basic types of sampling plans
are:
▶ Intuitive or
judgmental
▶ Systematic
▶ Random

Types of ▶ Hybrid plans based on a c ombination

of these approac hes are also used.
▶ Mandated plans may be needed – where
the sampling plan is specified by regulation
Samplin ▶
and must be followed exac tly.
Statistic al proc edures may be used to

g Plan determine how many samples are needed

to ensure c onclusions are based on
probability rather than personal
judgement. (Special expertise may be
needed to apply statistical proc edures to
develop sampling plans.)

40
 ▶ The intuitive or judgmental
approac h generally uses the
smallest number of samples but
involves the most bias in sampling
site selec tion.

▶ Sites are chosen based on prior history

Intuitive of the site or visual assessment.

Samplin ▶ Bec ause of the high bias in

c hoosing samples, the use of
sample results for litigation may
g Plan be limited.

▶ One sample taken just downstream

of an outfall is an example of
judgmental sampling. This one
sample may have a higher
c oncentration of the parameters in
question than the stream would be
expected to have.
41
 ▶ A random sampling plan uses
the largest number of samples
Random and generally involves the
least amount of bias.

Samplin ▶ Costs are usually high because

of the large number of
g Plan samples needed to c over the
site.

42
 ▶ A systematic sampling plan
uses a consistent grid or other
pattern.

▶ The number of samples and

therefore the resulting bias
Systemati are in between those for
intuitive and random plans.
c The c osts are intermediate
Sampling as well.

Plan ▶ Often a c ombination of intuitive

and random approac hes is the
best c ompromise between low
bias and fewer samples (i.e.,
lower cost).

43
 ▶ Complic ations in the sampling
proce ss occur from space or
time dependencies of the
proc ess or area sampled.
▶ Sampling loc ation must also
take depth into ac c ount.
Proc ess effluents are rarely
Samplin
▶
homogeneous. As a result, 3
samples for suspended solids
g taken from the top, middle,
and bottom of a stream may
Depth ▶
show greatly varying results.
The sampler may need to find
a way to mix samples
appropriately so that the
sample submitted for analysis
is representative of the stream.

44
 ▶ The time fac tor be comes
important when one c onsiders
that most pollutants do not
remain stationary. They move
▶
or mix.
Sampling must c onsider
Samplin the migration of
parameters.
g Times ▶ Another c omplic ation arises
when sites sele cted as part of
and Sites a grid are not readily
ac c essible or are not usable
for reasons of safety or power
requirements.
▶ Judgment may be needed to
move a pre-sele cted site using
the random or systematic
approac h to a different
45
loc ation.
 ▶ When c hoosing sites, safety
must be considered.

▶ Samples taken from sewers

Safet involve following the Highway
Traffic Ac t and procedures for
y c onfined space entry.

Issues ▶ Samples taken from a

waterc ourse may involve
boating safety.

46
 ▶ All prote ctive equipment must
be budgeted for and
provided.

▶ Samplers must be trained in

the use and maintenance of
this safety equipment.

Safet ▶ If hazardous materials are

y known to be present, material
safety data sheets (MSDS)
must be provided.
Issues
▶ Based on the data in the
MSDS, appropriate c lothing
and prote ctive equipment
should be used.

47
 ▶ The sampler must be aware of
the regulations under whic h
the sampling is being
Does the regulation c all for
conducted.
simple grab samples (one
shot) or c omposite samples
generally taken over a 24 hr
Regulatory period?
Requirement ▶ If c omposites are required,
s automated samplers may
be needed for some
parameters.
▶ The program c hief must ensure
that all samplers are fully
trained in the operation,
c alibration and maintenanc e
of these automated samplers.
48
 ▶ The regulation may also
spe cify the sampling
c ontainers, methods of
preservation and methods of
▶
sample
The handling
program and
c hief transport.
must
ensure that samplers are
Regulatory aware of these and are
Requirement properly trained.

s ▶ QC samples suc h as
bac kground samples (upwind
or upstream), instrument blanks
(wash water), c ontainer blanks
(empty c ontainers) may have
to be taken and doc umented
to meet the requirements of a
regulation.
49
 ▶ If samples will be used for
litigation, then c hain-of-
c ustody proc edures must be
in plac e and all staff must be
trained in their use.
▶ The sampler must ensure that
the sampling devic e and the
Litigatio final samples c ould not have
been tampered with.
n ▶ If automated samplers are
used, they should be in
Samples limited ac c ess areas (i.e.,
loc ked sheds).
▶ They should be visited
regularly to ensure that no
unauthorized entry has been
made and that the instruments
are working properly.
50
 ▶ These visits and observations
must be documented.
▶ Final samples should be
sealed either using paper
seals (c alled C ustody Seals)
over the mouth of the
Litigatio c ontainer or they should be
kept in loc ked boxes.
n ▶ The chain-of-c ustody must
be tracked.
Samples ▶ This c an easily be done with
pre- designed forms.
▶ The laboratory c hosen must
also maintain the chain-of-
c ustody after samples are
delivered.
51
 ▶ There are times when
field observations are
vital to a sampling
program.

▶ These may inc lude weather

Field data, flow data, types of
organisms or vegetation being
Observation studied and sightings of
s potential pollution sourc es
suc h as outfalls or drums.

▶ Pre-printed observation sheets

are an easy way to deal with
this need.

52
 ▶ Field testing is also
used extensively.
▶ Temperature, pH, and dissolved
oxygen are probably the most
analyzed parameters in the field,
but c hlorine, nutrients, and

Field some metals c an also be

analyzed using field test kits.

Testin ▶[Link]

▶ Samplers must be trained in

g the use of these instruments
and kits and understand their
limitations.
▶ If analyzed and documented
properly, these data are
perfe ctly valid for litigation.
53
 ▶ So far, we have dealt only
with setting up the field
sampling program. After the
samples are c olle cted, they
will have to be analyzed by
▶
a laboratory.
The laboratory c hosen must first
be c apable of analyzing the
Laborator types of samples c olle cted to
the level of performance
y needed.

Selection ▶ E.g., a lab that specializes

in determining metals in
drinking water may not be
capable of determining
c yanide in mine tailings.
▶ The performanc e of the
laboratory must be c onsidered.

54
 ▶ There are many exc ellent
labs doing mine assays at
high c oncentrations (i.e.,
perc ent levels) but
analyzing samples at the
ppb or ppt levels is vastly
different.
Laborator
▶ If very low dete ction limits or
y ce rtain performance criteria
are required by drinking
Selection water guidelines or
regulations, then these
laboratories may not be
c apable of meeting the data
quality objec tives (DQOs).

55
 ▶ A c hosen lab that does not
offer the full range of analyses
needed for a specific contract
will have to sub contrac t some
of the work.

▶ This c an pose problems with

Laborator turn- around times, quality,
and c osts – sinc e you no
y longer have dire ct c ontrol
over all of the proje ct.
Selection
▶ Multiple labs may also cause
a break in the c hain of
c ustody so that litigation
may be affec ted.

56
 ▶ Where sampling is being
c onduc ted to verify
c omplianc e with a regulation
or a c ontrol order, ensure that
the lab is using
methodologies permitted by
the regulations.
Laborator ▶ The regulations often stipulate
not only the methods of
y sample preparation and types
of instrumentation to be used
Selection but also the performanc e
expe cted.

▶ The laboratory must show

that it c an meet the
regulatory requirements.

57
 ▶ Some regulations require that
the laboratory be accredited
(Standards C ouncil of
▶
C
Toanada).
be ac c redited, a lab must
meet standards for
performance (PE or PT
Laborator samples), have training
programs, documented
y methods, means of trac king
samples, and even meeting
Selection c leanliness c riteria.
▶ Hiring an accredited lab will not
guarantee good analytic al
results, but it provides a
starting point.
▶ Laboratories must be lic ensed
by Ontario MOE to analyze
58
drinking water samples.
 ▶ Samples c an be c olle cted
manually or with
automated samplers.
▶ Automated samplers are
c ommonly used be cause of
Sample their c ost effe ctiveness,
versatility, reliability,
Collection performanc e and c ost.
Automate ▶ They are also the method of
d or c hoic e when safety is a
c oncern (i.e., c onfined
Manual spac e).
▶ Manual sampling is well suited
to a small number of samples
but is c ostly and time
c onsuming for routine and
large sampling programs.
59
 ▶ Initial response to c itizen
c omplaints of partic ulate
fallout or foul drinking water are
times when manual sampling
are used.
Sample ▶ Here the sampler is basic ally
trying to find the source of the
Collection complaint.

Automate ▶ A single sample c an be used

to determine the c ause of
d or the problem.
Manual ▶ Multiple samples taken from
various locations are needed
to determine the extent of
the problem.

60
 ▶ When multiple samples are to
be taken at frequent intervals,
or when a single sampling point
is to be sampled for an
Sample extended time, automated
samplers are put into use
Collection bec ause the manpower
Automate requirements to sample
manually are too high.
d or
▶ A human sampler taking
Manual samples has one great
advantage over an automated
sampler: visual observation.

61
 ▶ While some automated
samplers c an c olle ct multiple
sub-samples for visual
inspec tion, estimates of
sample variability (flow and
Sample characteristics) may be lost.
Collection ▶ A manual sampler has some
Automate extra flexibility to c ollec t
different types of samples
d or whenever needed.
Manual
▶ Automated samplers
generally don’t have this
flexibility.

62
 ▶ Certain sample types aren’t
easily c olle cted by automated
Sample samplers.
Collection ▶ Samples with large amounts of
Automate oil and grease, or samples
with partic ulates whic h may
d or c log the intake are generally
Manual not suitable for automated
samplers.

63
 ▶ Manual sampling depends on
the sample type, the c onditions
and equipment present and the
needs of the lab. Several types
are:
▶ Air partic ulates: razor

Sample blades, c otton swabs,

adhesive tape, glass or
Collection aluminum plates.
▶ Soil, sediment, solids in drums:
c alibrated scoops, c orers,
augers
Equipmen ▶ Liquids in drums: glass tubes,
t pole with multiple bottles
atta ched
▶ Water c ourse: dipper, extended
pole with sample bottle
atta ched, peristaltic pump,
messenger a ctivated sampling 64
bottle
 ▶ Water samplers fall into three
main types;
1) Vacuum samplers consist of an
evac uated c omposite
sample container with an
Water electrically or mechanically
operated pinch valve and a
Sampler ▶
length of tubing.
When the pinch valve opens,
s water is drawn into the
previously evac uated
c ontainer by the vacuum.
▶ The time the pinch valve is
open is set to deliver the
required amount.
65
 2) The peristaltic pump sampler is
the most used sampler.

▶ It uses a peristaltic pump to

Water transfer water from a sample
stream to a container via a
Sampler tube.

s ▶ A timing mec hanism c ontrols

the intervals between
portions and the size of the
portions c ollec ted.

66
 Water 3) Mechanical samplers use
some c ombination of wheels,
disks, or rotating scoops to
Sampler deliver water to a storage
container.
s

67
 ▶ For safety, maintenanc e,
reliability and sec urity in field
applic ations, the following
features are desired in an
automated sampler:
▶ Water tight c asing to
withstand total immersion
Vandal proof c asing with
Water
▶
provision for loc king

Sampler
▶ A sec ure harness or
mounting devic e if to be
used in a sewer
s ▶ Explosion proof c onstruction
▶ Capable of operating on AC or
DC
▶ C ompac t and portable for 1
person installation (under 20
kg)
68
 ▶ Variable sample collection interval
▶ C apable of flow proportional
and time c omposite samples
▶ Capable of collecting a single
large sample (10L) or 24 or
more disc reet smaller
samples

Water ▶

▶
Adjustable intake veloc ity
Minimum lift of 6 m
Sampler ▶ Manual c ontrol for test
c yc le operation
s ▶ No metal parts in c onta ct
with sample source
▶ Capable of temperature
control
▶ Purge c ycle
▶ Easily repaired and
a cc essible supply of spare
parts 69
 ▶ As a general rule the amount
of tubing needed to transfer
the sample from the water
sourc e to the storage
c ontainer should be

Water ▶
minimized.
This is especially important when
sampling for organic
Sampler parameters.
▶ Any tubing used should be inert
s to the materials being collected
(i.e., some types of plastic s
c ontain organic compounds
that can leac h into the sample
as it is collected.

70
 ▶ Automated samplers for air
monitoring generally work by
having a pump draw air
through some sort of filter or
sorbent material.
Air ▶ The filters may be a glass
fibre or other matrix either
Sampler alone or impregnated with a
sorbent.
s ▶ These filters c an be used to
determine the amount of total
suspended particulate in the
air, total c arbon, sulfur, and
metals.

71
 ▶ Solid sorbents suc h as tenax
and charcoal are used to trap
volatile organics.
▶ Most samplers have some sort
of mec hanism to limit the
Air size of particles trapped.

Sampler ▶ This is done in some c ases

to imitate the human

s ▶
respiratory tract.
Many of the features of water
samplers apply to air samplers
as well.

72
 ▶ Se curity, ease of
maintenanc e, portability,
adjustable sample volume and
number of samples, manual
test c yc le, no metals in

Air c ontac t with the sample flow

are attributes to c onsider.

Sampler ▶ Suc h samplers c oncentrate

the sample during c olle ction,
s be cause the volume or mass
of sample c olle cted on the
filter or sorbent material is
muc h less than the volume of
air sampled.

73
 ▶ There are 2 general types of
samples: grab and
c omposite.

▶ The selection of sample type is

Grab governed by the information
sought, the purposes of the
Samples / sampling, the analyses to be
performed, and the flow
C omposit pattern.
e
Samples ▶ A grab sample is defined as an
individual disc reet sample
collected at one place and at
one spec ific time or over a
period not to exc eed 15
minutes.
74
 ▶ A grab sample c an be taken
manually using any of the
devic es previously mentioned.

Grab ▶ For water samples, grab

samples are frequently
Samples / c olle cted when
the flow pattern is intermittent
C omposit ▶

▶ the water c hara cteristic s

e are constant
samples may be hazardous
Samples
▶

▶ samples may c hange with

storage
▶ Only maximum or minimum
data are needed

75
 ▶ Samples are to be analyzed
for oil and grease or
volatiles
Grab ▶ Samples are c olle cted
Samples / to monitor batc h
discharges
C omposit
e ▶ C orroborate
c omposite sample
Samples data

▶ If required by
regulation
76
 ▶ A c omposite sample is defined
as a sample formed by mixing
disc reet (grab) samples
c olle cted over periodic points
in time or a c ontinuous
▶
proportion
The numberofofthe flow.
grab samples
C omposit depends on the variability of
the c oncentration and flow.
e ▶ A c omposite sample
represents average c onditions
Samples for the given duration, usually
24 hours.
▶ This type of sample
requires a greater amount
of time and is often
c olle cted with an
automated sampler.
77
 ▶ There are two main types
of c omposite samples:
▶ Simple c omposite
▶ Flow proportional

C omposit ▶ All grab samples used to make

a simple c omposite have the
e same volume and are
Samples collected at a fixed time
interval.
▶ This kind of composite is used
when the c oncentration of
the analytes and the flow
are quite constant.

78
 ▶ There are two main types
of c omposite samples:
▶ Simple c omposite
▶ Flow proportional
C omposit
e ▶ Samples c olle cted by a
flow proportional system
Samples are c olle cted eac h time
the flow of the sampling
stream reaches a ce rtain
flow rate.

79
 ▶ Biological, chemical, and
physical changes may occur
after a sample is collected, that
change the sample’s
▶
c omposition.
Samples must be handled in a
manner to minimize these
Sample c hanges and to prevent
external contamination.
Preservatio ▶ The most c ommon c hanges in
n a sample between sampling
and analysis are a result of
volatilization, adsorption,
diffusion, prec ipitation,
oxidation, photoc hemic al
c hanges, and microbiological
degradation.

80
 ▶ Volatilization refers to the
physic al proc ess in whic h
volatile spec ies are lost to the
▶
atmosphere.
This proc ess depends on the
vapour pressure of the
analyte, the temperature of
Decompositio the sample and the surface
n & area.
Degradation ▶ A well sample suspe cted of
being c ontaminated by
Processes gasoline may lose
c omponents suc h as benzene,
toluene, and xylene through
volatilization.
▶ This is eliminated by c ontaining
the sample in a bottle with no
air or headspace.
81
 ▶ Metals c an be irreversibly
adsorbed onto glass
▶
surfac [Link] adsorbed
Oils are
onto walls of plastic
c ontainers.
Decompositio ▶ Organic molecules such as
n & plastic izers diffuse or migrate
out through plastic walls or
Degradation bottle caps.
Processes ▶ Ground water on c ontac t with
oxygen will often undergo
c hanges in whic h dissolved
iron will prec ipitate out as
solid iron oxides or hydroxides
or sulfide will oxidize to
sulfate.
82
 ▶ Light c an often degrade c ertain
organic c omponents suc h as
polycyclic aromatic
hydrocarbons (PAHs).

Decompositio
▶ Samples may c ontain
n & organisms that may degrade
Degradation organic components.
Processes
▶ For example, there are
bac teria that dec ompose
phenolic compounds.

83
 ▶ Preservation tec hniques often
involve the addition of a
c hemic al whic h ‘ties up’ the
analyte in a form whic h is less
affec ted by sample aging or
else provides c onditions
unsuitable for further reaction
Sample to occur.
Preservatio ▶ In some c ases, refrigeration or
n freezing to reduce reac tion
rates provides the best
preservation, espe cially for
those parameters which have
a direct biological
relationship (with respec t to
growth or dec line).
84
 ▶ Preservation for some
analytes is effective.

▶ For others, it serves only to

marginally reduce the de cay
Sample or c onversion rate.
Preservatio
n ▶ Therefore, it is essential for
such analytes as phenol and
chlorophyll that the samples be
submitted to the lab as quic kly
as possible to minimize any
loss.

85
 ▶ The sampler should be aware that
the use of the recommended
preservative for one parameter
may negate the possible
determination of another.
▶ E.g., a sample for heavy metals
preserved with nitric ac id is
now unsuitable for pH and
Sample nitrate tests.
Preservatio ▶ It is the sampler’s responsibility
to determine whether the use of
n a c ertain preservative will
eliminate the possible
determination of another
required parameter, and provide
a suitable replicate sample for
the sec ond parameter.
▶ Eac h replica te should have the
preservative used c learly marked
on the sample container label.
86
Sample
Preservation

87
 ▶ Just as important as
preservatives in minimizing
analyte c hange is the sample
▶
or shipping
Selec c ontainer.
tion of sample
c ontainer is also determined
by the volume required for
Sample analysis.

Container ▶ If c ontainers are prepared by

the laboratory, the sampler
s must ensure that the
c ontainers are c lean and
have been properly prepared.
▶ This may include pre-labeling,
pre- charging with preservative,
and capping tightly.

88
 ▶ If the lab is not preparing
sample bottles, the sampler
must ensure that it is done.

Sample ▶ Sample c ontainers, taken at

Container random, should be analyzed
to ensure that there is no
s c ontamination present from
the c ontainer or preparation
procedure (c ontainer
proofing).

89
 ▶ Some general guidelines
to selec tion of
c▶ontainers:
C onventional parameters in
water matric es (i.e., pH,
hardness, nutrients) c an be
Sample c ollected in 500 mL plastic
c ontainers. Avoid plastic s
Container whic h ‘breathe’ since
parameters suc h as ammonia
s may c hange signific antly in
transit.
Sludge samples should never be
filled more than half way to
allow for gas formation. Trac e
metals and c yanide are
c ollected in the same type of
plastic c ontainer.
90
 ▶ Solid samples for any of the
conventional or trace metal
parameters may be c olle cted
in either wide mouth plastic or
Sample glass jars or even plastic bags.

Container
▶ Some solid samples suc h as
s vegetation should be dried
as quic kly as possible to
prevent decay.

91
 ▶ Organic parameters are
c ollec ted in glass c ontainers
regardless of the matrix.
▶ The lids of these containers should
be lined with teflon or aluminum
foil.
Do not use plastic bottles for
Sample
▶
organic parameters since low
level contamination may occur.
Container ▶ As a worst c ase, plastic bottles
s c ontaining organic solvents
have ac tually dissolved before
getting to the lab for analysis.
▶ Samples for volatile parameters
must be collec ted and stored
with no headspace (air) in the
containers.
92
 ▶ Air filters are normally
transferred to the lab folded
over in envelopes to minimize
loss of any trapped
partic ulates.
Sample ▶ If the filters need to be stored
Container for an extended time, they
should be stored at low
s humidity.

▶ Solid sorbents suc h as tenax

are sealed for transit to the
lab.

93
Sample
C ontainers

94
 ▶ After sampling and
preservation, the samples are
ready for transport to the lab.

▶ Samplers must be aware of

any provinc ial or federal
Sample regulations c ontrolling the
transport of hazardous goods
Submissio and ac t ac c ordingly
(Transportation of Dangerous
n Goods, TDG).

▶ While dire ct delivery by the

sampler is the best method,
this sometimes not practical
or possible.
95
 ▶ Third party c arriers, suc h as
c ouriers, priority post or bus
express c ompanies all c arry
lab samples however they
make no effort to refrigerate
Sample samples or keep them from
being jostled.
Submissio ▶ As a result, some samples
may deteriorate.
n
▶ For legal samples, the
fewer people involved,
the better.
▶ Couriers must sign the
c hain of c ustody form.

96
 ▶ All samples should be
labelled with the following
information:
▶ Sample ID. This may include
loc ation identifiers, date
identifiers, or a simple
numbering system.
▶ Sample loc ation desc ription
Sample (e.g., River X, 50 m
downstream of outfall)
Submissio ▶ Presence of any chemical
preservative
n ▶ Indication of the test requests for
that bottle
▶ Samples whic h c ontain or
are suspected of containing
hazardous materials should
be labelled for the
protec tion of laboratory
staff.
97
 ▶ Fish samples for metals or
merc ury determinations are
plac ed in plastic bags and
▶
frozen. for PCB or pestic ide
Samples
Sample analysis are wrapped in
solvent washed aluminum foil
Container and frozen.
s ▶ Generally only fish filets
are submitted.
▶ Any knife used to c ut the
filets must be solvent washed
as well.

98