Standard Operating Procedure

for Collection of Water and

Wastewater Samples
Comprehensive Guide for Effective Sampling Techniques
Module-1
What is Sampling
• Sampling involves collecting a portion of material or aliquot for
analysis, ensuring it represents the material accurately.

• Relative proportions or concentrations of pertinent components should

remain the same in the sample as in the original material.

• Handle samples to prevent significant changes in composition before

testing.
 Scope of Water Sampling
• Comprehensive Monitoring: • Early Warning Systems:
• Surface Water: Rivers, lakes, reservoirs. • Real-time monitoring.
• Groundwater: Underground sources. • Prompt detection and preventive measures.
• Wastewater: Treatment plants, industrial • Water Management Support:
discharges.
• Sustainable resource management.
• Regulatory Compliance: • Policy formulation based on data.
• Adherence to standards and guidelines.
• Support for legal enforcement actions.
• Research and Development:
• Innovative sampling methods.
• Environmental and Public Health: • Support for scientific studies.
• Pollution control.
• Ensuring safe drinking water. • Community Awareness:
• Educating the public.
• Data Collection and Trends: • Providing accessible data.
• Database development.
• Long-term and short-term trend analysis.
Scope of Water Sampling
· Where to take sample
· When to take samples
· How to take samples
· How many samples to take?
· How often the samples will be taken
· How much sample is needed?
· How to preserve the samples?
· How long the samples will be stable?
· What to take (air, soil, water)
· What are the parameters to be analyzed
· Who will take samples (sample custody)?
 Objectives of the Water Sampling
Samples are presented to the laboratory for specific determinations and the sampler being responsible for collecting a
valid and representative sample to fulfill the following objectives
o To gather information such as location, source of water, depth, length, nearby industries etc. about the water
body from which the representative samples are drawn.
o To identify the state and trends in water quality, both in terms of concentration and effects.

o To identify the mass flow of contaminants in surface water and effluents.

o To formulate the Standards and permissible limits of pollutants.

o To demonstrate whether continuing compliance with specific regulatory requirements have been achieved.

o To warn early and detection of pollution.

The above objectives of sampling can be only ensured by adopting the appropriate technical & scientific procedure of
sampling, proper preservation and transportation of collected samples. A Representative sample should be drawn to
yield insights and observations of pollution surrounding the problem area to produce a qualitative analysed report.
Following procedures are to be followed for performing the correct sampling.
Table-I SAMPLING AND HANDLING REQUIREMENTS

Parameter Container PRESERVATION MAX.STORAGE

Acidity P,G Refrigerate 24 h
Alkalinity P,G Refrigerate 24h
BOD P,G Refrigerate 6h
Boron P,G HNO3 to pH <2 28d
Carbon, Total G(B) Analyse immediately or 7 days
add HCl to pH<2
Carbon dioxide P,G Analyse immediately 15 min
COD P,G Analyse immediately or 7 days
add H2SO4 to pH<2,
refrigerate
Chloride P,G Refrigerate --
Chlorine, residual P,G Analyse immediately 15 min
Chlorophyll P,G Unfiltered, dark, 4’C 48 hours
Colour P,G Refrigerate 48 h
Conductivity P,G Refrigerate 48h
Cyanide, Total P,G Add NaOH to pH>12, 24 h
refrigerate in dark
Fluoride P -- 28 days
Hardness P,G Add HNO3 to pH<2 6 months
Metals, General P(A),G(A) Add HNO3 to pH<2
Metals, Dissolved, P(A),G(A) Filter immediately, add
General HNO3 to pH<2
Chromium VI P(A),G(A)
Nitrogen, Ammonia P,G Analyse immediately or 7 days
add H2SO4 to pH<2,
refrigerate.
Nitrogen, Organic P,G Refrigerate, add H2SO4 7 days
to pH <2.
Nitrate P,G Analysis as soon as 48h
possible, refrigerate
Nitrite P,G Analysis as soon as --
possible, refrigerate.
Nitrate+Nitrite P,G Add H2SO4 to pH<2, 2 days
refrigerate
Oil & Grease G(S),Wide Add H2SO4 to pH<2 28 days
mouth
Oxygen, dissolved G Analyse immediately 15 minutes
Pesticides G(S) Refrigerate, add 7 days
ascorbic acid if residual
chlorine is present
Requirements for water sample collection and Field
kit preparation selection of sample containers
• The desired appliances/ equipment/chemicals are to be carried along with the qualified and trained manpower.
The following major facilities are required for water sampling:
 Thermometer and handy/portable pH, DO and conductivity meters.
 Amber, wide mouth glass bottles and plastic cans (PE/TEFLON) of 1-2 L capacity and BOD bottles/glass vials.
 Sodium hydroxide, Con. H2SO4, Con. HNO3 and Zinc acetate for preservation.
 Ice Box/Crate for transportation of samples.
 Marker/indelible ink pen for labelling of containers.
 Ensure that all sampling equipment is clean and quality assured before use.
 Bake at 450oC bottles to be used for organic analysis sampling.
 Stainless steel bucket with nylon rope.
Grab sample
• A grab sample is a single sample taken at a specific time.

• Most common type of sample used in labs.

• Example: Collecting a beaker of raw water and testing it for pH.

• Limitations: Represents a snapshot of water characteristics at a specific point and time.

• Most suitable for small plants with low flows and limited staff.

• Preferred for tests that need immediate analysis: pH, dissolved oxygen, and total residual chlorine.

• Must be collected carefully to be as representative as possible.

• Should be taken when the plant is operating near its average daily flow rate.

• Effluent samples should be delayed to allow raw water to pass through the treatment process.

• Mixing grab samples may alter pH and chlorine residual values due to chemical reactions.
Composite sample
• Composite samples, or integrated samples, are mixtures of several grab samples.

• Collected at regular, specified time periods in proportion to flow.

• Provide a more representative sample of water characteristics over time.

• Strength: Account for changes in flow and water characteristics over time.

• Help operators understand the overall effects of influent on treatment and effluent
on receiving water.

• Not suitable for tests of water characteristics that change during storage.

• Not suitable for tests of water characteristics that change when samples are mixed,
like pH.

• Composite samples are often taken using automatic sampling devices. These may
be set to take a sample every 8, 12, or 24 hours.
• The frequency depends on test requirements, the size of the treatment plant, and
permit requirements.
• Composite samples are taken automatically every 8, 12, or 24 hours, based on test
needs, plant size, and permit requirements.
Composite sample
Sample Volumes for Composite Samples
• Each grab sample in a composite must be proportional to the flow at the time of
collection.
• Automatic equipment typically calculates and collects correctly sized grab
samples.
• Sample volume depends on the flow volume at collection time, total daily flow,
total composite sample volume, and the number of grab samples.
• The following equation can be used to calculate a grab sample's volume.
Composite sample example
• For example, the average daily flow at your plant is 11.3 MGD and the total volume of your composite
sample is to be 4,000 mL made up of 24 grab samples. At the time you take your first sample, the plant's flow
is 5.2 MGD, so you can calculate the volume of the grab sample to take as follows:

• So, you should take a 77 mL grab sample during your first sampling of the day.
Example
To collect an 8-hour composite sample with a 2-hour interval, five samples would be needed. If a total sample
of 2 liters was needed, the average daily flow was 60,000 gallons, and the flow at the first sample time was
45,000 gallons per day, determine the composite sample single portion size needed, in Liters.
Storage
• Analyze all samples as soon as possible after collection for best results.

• When immediate analysis isn't possible, store, preserve, and treat samples before testing.

• Follow specific guidelines for permissible storage duration and correct preservation techniques for
each test.
Sampling Methods

• Manual Sampling: Requires trained technicians, minimal

equipment, and is essential for complex sample collection;
often used for regulatory and research investigations and for
collecting samples like waters containing oil and grease.
• Automatic Sampling: Reduces labor costs and human error,
allows for more frequent sampling; must ensure sampler
compatibility with sample constituents to avoid contamination.
• Sorbent Sampling: Increasingly used for rapid, inexpensive
sampling; effective if analytes can be adsorbed/desorbed
efficiently and if water matrix is free of particulates.
Types of Samples: Grab Samples
• Grab Samples: Single samples collected at a specific spot
over a short period (seconds or minutes)
• Represent a "snapshot" in space and time
• Discrete grab samples: taken at a selected location, depth, and
time
• Depth-integrated grab samples: collected over a predetermined
depth at a selected location and time
• Use Cases:
• Relatively constant composition sources: protected groundwater,
treated water supplies, well-mixed surface waters
• Not suitable for varying sources: wastewater streams, rivers, large
lakes, shorelines, estuaries, groundwater plumes
Types of Samples: Composite
Samples
• Composite Samples: More representative of heterogeneous
matrices with varying analyte concentrations
• Combining portions of multiple grab samples
• Using automatic sampling devices
• Sequential (time) composites: Continuous sampling or mixing
equal water volumes at regular intervals
• Flow-proportional composites: Continuous pumping proportional
to flow or mixing volumes based on flow rates
• Advantages:
• Reduced analysis costs, more representative samples, larger sample sizes
• Disadvantages:
• Loss of analyte relationships, potential analyte dilution, increased analytical
interferences, reduced statistical validity
Composite Sample
Considerations
• Avoid using composite samples:
• For components changing during storage: dissolved gases,
residual chlorine, soluble sulfide, temperature, pH
• Analyze individual samples ASAP after collection
• Sampling Method:
• Collect portions in wide-mouth bottle hourly or more
frequently, mix at end or combine as collected
• Use preservatives initially if needed
• Automatic Sampling Devices:
• Avoid unless samples are preserved
• Routine cleaning required for extended periods
Multiple-choice questions (MCQs)
1. What is the primary objective of water sampling?
a) To reduce the water level in reservoirs
b) To ensure that the sample accurately represents the material being sampled
c) To increase the chemical reactions in water samples
d) To change the composition of the water sample
2. Which of the following is NOT a source from which water samples are
typically collected?
a) Surface water sources like rivers and lakes
b) Groundwater sources
c) Space stations
d) Wastewater from treatment plants and industrial discharges
3. Why is regular and systematic sampling crucial?
a) To reduce the cost of water management
b) For trend analysis and early detection of pollution
c) To increase the speed of water flow
d) To decrease the amount of data collected
Multiple-choice questions (MCQs)
4. What should be considered when deciding the timing of water sampling?
a) The color of the water
b) Typical conditions of the water body and specific events like rainfall
c) The temperature of the sampling equipment
d) The location of nearby restaurants
5. What is a critical factor in preserving the integrity of collected water
samples?
a) Exposing the sample to direct sunlight
b) Ensuring proper preservation and transportation
c) Mixing the sample with other chemicals
d) Storing the sample at room temperature indefinitely
6. What is the role of qualified personnel in the sampling process?
a) To take samples without any documentation
b) To collect samples and follow proper documentation and chain of custody protocols
c) To randomly select sampling locations without consideration
d) To ignore the preservation of samples after collection
Multiple-choice questions (MCQs)
7. Which of the following is NOT listed as a requirement for water sample collection?
a) Thermometer and pH meter
b) Amber glass bottles and plastic cans
c) Aluminum foil for sample wrapping
d) Sodium hydroxide and zinc acetate for preservation

8. What is the primary advantage of using grab samples for water testing?
a) They provide a snapshot of water characteristics at a specific time.
b) They represent the entire flow of the water body.
c) They are always more accurate than composite samples.
d) They eliminate the need for manual sampling.

9. Which method is recommended for obtaining a representative sample over time in a heterogeneous matrix?
a) Grab sample
b) Discrete sample
c) Composite sample
d) Sorbent sample

10. Why is it important to avoid using composite samples for tests of dissolved gases, residual chlorine, and pH?
a) These characteristics do not vary over time.
b) Composite samples may change significantly and unavoidably during storage.
c) Composite samples are easier to preserve.
d) These characteristics are better measured using sorbent sampling.