Freshwater Management 7BY507

Sampling & Analysis

Dr Laura Chan

derby.ac.uk
At the end of this session, you will be able to:

• evaluate key considerations needed in

planning to sample and analyse a
freshwater body

• describe different field and/or laboratory

techniques available to analyse water
samples

• critique sampling and analytical techniques

in order to produce reliable results

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Sampling Strategy for freshwater bodies
• Planning a sampling strategy is key, so data is
representative of an area to build an overall
picture.

• Variables must be considered, e.g., seasons,

and weather.

• Costs/time can limit the number of samples.

• The design aims to produce unbiased, reliable

and sufficient data which can be interpreted
statistically.
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Considerations for a sampling strategy - whiteboard

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 Key considerations
• What samples to take?
• How many samples to take?
• How many replicates are needed?
• How to ensure the samples are representative?
• What costs are involved?
• How much money is allocated for the study?
• What to analyse for?
• How to record the data?
• Safety?
• Permission to take samples?

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Record Keeping

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 Sampling systems

The type of sampling system depends on what the

study involves and the type of study site.

• Judgemental sampling - where a discharge point is

known, and sampling is concentrated in that area.

• Systematic sampling uses a grid or transect line to

take regular samples following a pattern.

• Random sampling is where locations are generated

using a computer programme

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 Sampling and storage of water samples
• Inorganic substances, Teflon bottles should be used.
For short term, high density polyethene (HDPE) are
cheaper.

• Organic chemical analysis, use dark-coloured glass

bottles to prevent reactions with sunlight and plastics.

• For bacteria determinations, use sterile containers and

aseptic techniques to prevent cross contamination

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 Taking water samples
• Initially, pots should be labelled with
permanent marker before taking the
samples.

• Rinse sampling bottle at least twice with

water at each sampling location, collecting
the third fill as the sample.

• Submerge just under the surface of the

water (up to 5 cm depth) to avoid collecting
floating fragments or oil.

• Bottles should be filled to the top to avoid

an air space and be capped tightly

https://youtu.be/t13XnjQhPlc derby.ac.uk
 Taking water samples from specific water bodies

• Lotic
• Take in main flow or use judgemental system
• Avoid disturbing sediments
• Different sampling depths may be required

• Groundwater
• From monitoring wells to pump water to the
surface.
• Allowed to flow for a few minutes before sampling
• Avoid contamination of groundwater

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 Storage and transportation of water samples

• Keep upright to prevent spillages.

• Keep cool to prevent microbial growth or volatile

organics undergoing transformations.

• Filter through a 22µm filter paper, for further

laboratory analysis.

• For metal analysis, acidify with a drop of

concentrated nitric acid to prevent microbial growth

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 Quality control in sampling

• Trip and field blanks https://youtu.be/8MORV4SVoMU

• Avoid cross contamination

• Consider accuracy and precision of your sampling

Activity 1: Drag and drop – Study Materials – Week 9

Match the definitions/applications into either accuracy

or precision

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Field testing to identify pollution in freshwater
pH
Indicates acidified water, pH <6
Indicates Alkaline water, pH >8

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pH tolerance of biota

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 pH Effect on Heavy Metal Release from a Polluted Sedim
ent (Zhang et al., 2018)
• “The performance of Cd, Ni, and Cu release from river sediment at different pH was
investigated by a leaching test using deionised water and river water as leachants”

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pH Effect on Heavy Metal Release from a Polluted Sedim
ent (Zhang et al., 2018)

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 Conductivity
Measured in µS/cm-1, the more salt ions present the higher
the conductivity.

If a higher-than-expected result is obtained, further

laboratory analysis can identify what ions are present.

This is used as an early indicator of heavy metal

pollution.

Deionised water = 0.5 - 3 μS/cm

Tap water = ~ 50 μS/cm
Freshwater = < 2000 μS/cm
Sea water = ~ 50,000 μS/cm

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 Dissolved Oxygen
Measured in mg/l of oxygen dissolved. It is important
to take the temperature of the water measured at the
same time.

Typical figure for freshwater at 15oC = 10mg/l

This measurement can be expanded upon in the

laboratory over some time to provide the biochemical
oxygen demand (BOD).

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 Total suspended solids (TSS)

Floating particles and colloids in water which do not

settle through gravity (particles that cannot be
removed with a 45 µm filter).

Secchi disc

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 Dipstick measurements
✔ Total alkalinity
✔ pH
✔Hardness
✔ Lead
✔ Copper
✔ Iron
✔ Mercury
✔Chromium/Cr(VI)
✔ Bromine
✔ Nitrate
✔ Nitrite
✔ Residual chlorine
✔ Fluoride
✔ Sulphite

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 Achieving reliable results from planning and analysis of water

Group Activity (20 mins)

• Reflect on what you have learnt so far and give two

positives and two negatives for sample planning and
any other considerations

• Post your thoughts on the Padlet board with your

group number.

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 Laboratory analysis of water

• For a more accurate and precise determination use

instrumental laboratory techniques.

• Atomic absorption spectroscopy (AAS) or inductively

coupled plasma spectroscopy (ICP) are typically used
for heavy metals.

• AAS can be used to determine over 70 different

elements.

• ICP can determine elements with atomic mass ranges 7

to 250 (Lithium to Uranium).

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 Anion determination
Anions are elements or a group of elements which form
negatively charged ions. Examples of freshwater pollutants:

• Phosphates (PO43-) and nitrates (NO3-) from

fertilisers
• Chloride (Cl-) from road gritting
• Naturally occurring fluoride or artificial fluoridation
(F-)

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 Ion chromatography (IC)
A form of liquid chromatography. Ionic species are measured by separation
through interactions within a column. Useful for anions.

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 Biological oxygen demand (BOD)
• Based on how much oxygen bacteria use in aerobic
respiration when breaking down organic waste.

• Conditions, e.g., temperature and pH of the

samples need to be controlled to keep the bacteria
‘happy’.

• Dissolved oxygen is measured initially and after 5

days.

• The more oxygen is depleted, the more organic

matter is in the water, which indicates a possibility
of sewage pollution

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Gas chromatography with mass spectrometry (GC-
MS)
• Used to identify many
organic pollutants, such
as oils fractions or
pesticides.

• GC separates the
components and
quantifies by size of a
peak.

• MS identifies any
unknown components

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 Other laboratory techniques

• Microscopy
• Scanning electron microscope

• Infra-red spectroscopy

• Liquid chromatography

• Nuclear magnetic resonance (NMR)

• Etc…

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 Laboratory Analysis Quality Control
1. Make use of composite samples.
2. Replicate analysis (a mean result can then be
reported).
3. Use a reagent blank and analyse this along with any
control blanks from sampling.
4. Prepare standard solutions to calibrate and measure
performance of any analytical instruments.
5. Use a certified reference material to calculate %
recovery of your analyte.
6. If a certified reference material is not available use
‘spiked’ samples.

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 Study Materials Week 9 - Group Activity 2 (30 mins)
• Select one of the techniques listed and either watch
the video (link in the folder) or use a method of
research. Or choose another technique used to
analyse water.

• List the type of water pollution which can be

identified. Add 2 advantages and 2 disadvantages of
your technique.

• Share your posts on the Padlet to inform your peers.

• Choose from AAS, ICP, BOD, IC or GC-MS or an

alternative if you wish.

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AAS video clip:
https://www.youtube.com/watch?v=_izbNvw2Tkg

ICP video clip:

https://www.youtube.com/watch?v=aCi72rj0fYA

IC video clip:
https://www.youtube.com/watch?v=Y4ap97fz478

BOD video clip:

https://www.youtube.com/watch?v=v33CgWJ2TZ0

GC-MS video clip

https://www.youtube.com/watch?v=bVKASwadjQY&t=1s

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