SAMPLING

PROTOCOLS,
PROCEDURES
AND SAMPLE
HANDLING
 COVERAGE
• Effluent Quality Monitoring Plan
• Quality Assurance and Quality
Control
• Sampling Techniques
• Standard Sampling Procedure and
Protocol
• Sample Handling
• Data Assessment and Validation
 EFFLUENT
QUALITY
MONITORING
PLAN
 EFFLUENT QUALITY MONITORING PLAN
Component of Monitoring Plan

• Objectives
• Background Information
• Monitoring Stations
• Effluent Quality Parameters for
Measurements
• Frequency of Monitoring
• Water Quality Sampling and Test Method
• Quality Assurance and Quality Control
Procedures
 PREPARATION OF EFFLUENT
MONITORING PLAN
• Objectives of monitoring
• Locations, type of industry and type of
WTP
• Number and location of discharge
outlet and permit conditions
• number of samples and parameters to
be analyzed
• In-situ analysis
• Sample preservation and holding time
 QUALITY
ASSURANCE
AND QUALITY
CONTROL
 QUALITY ASSURANCE AND
QUALITY CONTROL

To meet the goals of sampling, the data

must be:

• Representative
• Reproducible
• Defensible
• Useful
Quality Assurance and Quality Control

Sources of Error
• Measurement Error
• Method Detection Limit
• Sample Handling Error
Quality Assurance and Quality Control

Quality Control Methods

• Equipment Calibration and
Maintenance

• Field Data Form and Chain of

Custody of Samples

• Samples must have appropriate

label
Quality Assurance and Quality Control

Quality Control Checks

Field Quality Control Samples

• Equipment blank
• Field blank
• Trip blank (VOC)
• Field Duplicates
• Split samples
• Blind samples
Quality Assurance and Quality Control

Prevention of Sample
from Contamination
• Field Measurement should always be
made on site
• Sample Container must be cleaned
according to the recommended
method
• Samples must be submitted to the
laboratory as soon as possible.
Quality Assurance and Quality Control

Prevention of Sample
from Contamination
• Preservatives should be freshly
prepared and dispensed using
clean glassware
• Recommended preservation
methods must be followed
Quality Assurance and Quality Control

Prevention of Sample from

Contamination
• The inner part of sample containers and
caps should not be touched with bare
hands, gloves, etc.

• Sample containers must be kept in a

clean location, away from dust, dirt,
fumes.

• Sample must never left to stand in the

sun
Quality Assurance and Quality Control

Prevention of Sample from

Contamination
• Sample containers which have been
sterilized for microbial sampling must
remain sterile until the sample is
collected.

• All foreign objects, specially metal

objects must be kept out of contact with
preservatives and water samples.
Quality Assurance and Quality Control

Prevention of Sample from

Contamination
• Specific Conductance should never be
measured in sample water that had earlier
been used for pH measurements.

• All sampling instrument, equipment,

containers, supplies and material to be
used in sampling should be packed in
clean containers before leaving for site.
Quality Assurance and Quality Control

Personnel Qualification
and Training
• Effluent monitoring activities should
always be undertaken under the direction
and supervision of persons in authority
who have the right educational
background, experience and qualification
in effluent monitoring

• Field personnel must be trained on every

aspect of effluent quality monitoring
before assigning them to effluent
sampling and related activities.
 SAMPLING
TECHNIQUES
 SELECTION OF SAMPLING
STATION
• Effluent
If the purpose of monitoring is to meet
the DENR requirements on Self Monitoring
Report

• Influent/Effluent of each treatment

unit
Intends to evaluate performance
efficiency of the treatment units
 BASIC CONSIDERATIONS IN
SAMPLING

• Representative
• Downstream of all treatment
processes
• Flow rate of the effluent can
be measured and estimated
• Accessible
FREQUENCY OF SAMPLING
• Monthly

• Quarterly

• As needed
 Effluent Quality Sampling
and Test Methods

• Method should be recognized by the

EMB
• Sampling procedures, containers,
and preservation technique should
conform to the selected laboratory
method.
Effluent Quality Parameters
for Analysis

• Effluent quality parameters for

analysis will depend on the type
of your industry (DAO 34)
Field Personnel

All personnel involved in effluent sampling

and data collection activities must have the
experience and skills to perform these
activities
 Coordination with the
Laboratory

• The parameters proposed for

analysis and number of samples to
be collected.

• The estimated time the sample will

be received at the laboratory.
SAMPLING AND FIELD TEST
METHODS AND TOOLS

Sampling Methods

• Grab Sampling
• Composite Sampling
SAMPLING METHODS

Grab Sampling

Manual
Technique used for collecting grab samples
for immediate on-site field analysis

Direct Sampling with the Sample Container

Sampling may be done using the sample container

which maybe a wide-mouthed glass container,
plastic container, BOD bottle, or vial with cover
SAMPLING METHODS

Grab Sampling

Dip Pond Sampler

Samples can be
obtained at
distances as far as
3 m from the edge
of the source
SAMPLING METHODS

Composite Sample

• Composite sample are preferred

when the concentration of the
parameter under consideration is
expected to vary with time
SAMPLING PROCEDURES

Composite Sampling
• Manual composite sample consist of
grab samples typically taken at
equally spaced time intervals and
combined or mixed when all sub-
samples have been collected.
• Automated composite samples can be
taken either proportional to the
wastewater stream flow or on an
equal volume/equal time method
 SAMPLING PROCEDURES
1. Put on protective gloves

2. Obtain a pre-labeled sample bottle and

remove the lid without touching the inner
surface of either the bottle or the lid

3. Rinse the container at least three times

with the effluent, except for container
with preservative and for sample intended
to be analyzed for Petroleum oil, animal
and vegetables fats & oil (AVFO), total
coliform or fecal coliform.
 SAMPLING PROCEDURES

4. Hold the bottle below the neck and

lower it into the effluent. Ensure that
the hands do not touch the bottle
opening. For samples to be analyzed for
oil and grease take samples only from
the surface of the water. Do not
submerge the sample bottle below the
water surface
 SAMPLING PROCEDURES
5. Slowly lift the container towards the
flow. Fill it to about 4/5 full.
Enough space should be left to allow
for addition of preservative, if
necessary, and to allow for mixing
the sample.

6. Cap or cover the container and place

sample in a cooler containing
sufficient quantity of ice.
 ON-SITE MEASUREMENTS
• On-site measurements of samples is
necessary to obtain actual concentration
of effluent quality parameters that might
change during transport to the
laboratory, or these parameters might
change due to some value adjustments
required in subsequent laboratory
analyses.
ON-SITE MEASUREMENTS

Temperature Measurement for

Facilities Discharging Hot Effluents
For Rivers

• Sample should be collected from

upstream of the source, few meters
before outfall
• Sample should be collected from
downstream of the outfall, before
mixing with discharges of other
sources.
Recording Field Observation

The Field book should be:

 hard bound
 not be discarded
 provided with page number

 have all entries written in

ballpen or permanent ink
 Recording Field Observation
Details recorded should include:
 those noted on the sample bottle
 type of samples collected
 kind of measurement done and how
those were taken
 the results obtained
 preservative used
 all supporting information
 adequate space should be available for
comments
 Field Data Forms and Labels
Field Data forms must include:
 date and time of sample collection
for each parameter tested
 names of collectors
 sample sites names or codes
 influent/effluent flows
 color and odor of the water samples
Field Data Forms and Labels
Sample Label:
 clean
 secured
 waterproof and non-smearing
 large enough for the facility
name and date
 STANDARD
SAMPLING
PROCEDURES &
PROTOCOLS
STANDARD SAMPLING PROCEDURES
& PROTOCOLS

• Coordination
Institutional recognition for travel
arrangements, sampling
arrangements (e.g. boat hire) and
transport of samples (if requiring
transport by air or sea);

Notification to the laboratory on the

expected date and time of sample
arrival;
STANDARD SAMPLING PROCEDURES
& PROTOCOLS
• For Documentation
Pens (not pencil, not sign pen),
clip board
Sample labels
Field notebook
Field Data Sheet, Chain of Custody,
Other forms
Digital camera or recorder for photo
documentation
GPS (if necessary)
 FIELD DATA FORM
Source:
Address/location:
Date of Sampled:
Type of Sample :

Remarks:____________________________________________________________________________

Samples Collected by: ____________________ Signature:__________________

Analyzed on-site by: _____________________ Signature:__________________
Conforme (Company Representative): _____________________ Signature:__________________
CHAIN–OF-CUSTODY
 STANDARD SAMPLING PROCEDURES
& PROTOCOLS
• For sampling
Sample bottles and covers, preservatives,
labels and marker pens, trash bags, wash
bottles, field laboratory wares (pipette,
beakers, Erlenmeyer flask, etc.)
Sample containers/ transit containers and
ice packs
Effluent Monitoring Plan
Samplers/ sampling equipment including
extension poles, if needed
SAMPLE CONTAINER
 STANDARD SAMPLINGPROCEDURES
& PROTOCOLS
 For safety

First-aid kit
Rubber gloves, or disposable vinyl
gloves, boots, etc
Material safety data sheets (MSDS)

Waterless hand wash or hand wipes

 STANDARD SAMPLING
PROCEDURES & PROTOCOLS
 For transportation

Vehicle with sufficient capacity for

personnel, supplies and
equipment

Road-worthiness of vehicle. Check battery,

lubrication, coolant, windshield washer

Sufficient fuel for the trip (either in the

tank, in fuel container, or availability of
gasoline stations along the route

Availability of spare tire, jack, wheel wrench,

early warning device, etc.
 EFFLUENT SAMPLING PROCEDURE
• Based on preliminary survey, locate
the facility’s outfall;
• Collect samples
(Based on Sampling Procedures)
• Rinse outside surface of sample
container;
• Conduct on-site measurement as
necessary;
EFFLUENT QUALITY MONITORING

Upstream
Plant
Influent

WTF

Effluent

Downstream
 Effluent Sampling in Typical
Treatment Facilities
• Biological Treatment
Effluent is normally taken from
the discharge of the last treatment
unit
• Ponds/Lagoon
Effluent samples can be taken from
the outfall right after the weir or
from its discharge outfall
 Effluent Sampling in Typical
Treatment Facilities

• Chemical Treatment
Sample is collected from the
discharge of the last
sedimentation tank
• Septic Tank
Collect sample at the effluent
filter at the last chamber
 Effluent Sampling in Typical
Treatment Facilities

• Chlorinated Effluents

Effluent sample is collected

from the unit following the
chlorine mixing tank
Table 2 Significant Parameters for Selected Types of Industries

Type of Industry Significant Parameters

BEVERAGE INDUSTRY BOD5, pH, SS, Settleable Solids, Oil-Grease

CEMENT, CONCRETE, LIME, pH, Suspended Solids, Dissolved Solids,

LIME & GYPSIUM Temp

LIVESTOCK INDUSTRY BOD5, COD, TSS, pH, Color, Total Coliforms

MINERAL ORE PROCESSING Suspended Solids, Heavy Metals (Hg, CN, Cd,
(MINING INDUSTRY) etc.), Arsenic
PETROLEUM REFINING BOD5, Heavy Metals, COD, Oil (total), pH,
INDUSTRY Phenols, SS, temperature, TDS
PULP AND INDUSTRY BOD5, COD, pH, TSS, E. Coli, Color, Heavy
Metals, DS, Oil-Grease, Phenols
SUGAR CANE PROCESSING BOD5, pH, SS, Oil-Grease
INDUSTRY

HOTEL/RESTAURANT/HOSPI BOD5, Oil-Grease, TSS, pH, SS, Temperature

TALS
GEOTHERMAL POWER Color, Chromium, pH, Phosphate, TSS,
PLANTS Nitrate, Temperature, Chloride, Cadmium,
Lead, Copper, Nickel and Zinc
 SAMPLE
HANDLING
 Summary of Special Sampling or Handling Requirements

Minimum Maximum Storage

Sample
Determination Container† Sample Size Preservation§ Recommended/
Type‡
Ml Regulatory||
pH P, G 50 g Analyze immediately 2 h/stat
Temperature P, G - g Analyze immediately stat/stat
BOD P, G 1000 G Refrigerate 6 h/48 h
TSS P, G 200 g, c Refrigerate 7 d/2-7; see cited
G, wide-
Add HCl to pH<2,
Oil and Grease mouth 1000 G(a), c 28 d/28 d
refrigerate
calibrated
Add NaOH to pH>12, 24 h/14 d; 24 h if
Cyanide P, G 500 g, c
refrigerate in dark# sulfide present
Metals, general For dissolved metals
6 months/6
(Pb, Cd, Cu, and P(A), G(A) 500 g, filter immediately, add
months
Zn) HNO3 to pH<2
Add HNO3 to pH<2,
Metal: Mercury P(A), G(A) 500 g, c 28 d/28 d
40C, refrigerate
 † P = plastic (polyethylene or equivalent); G = glass; G(A) or P(A) = rinsed with 1 + 1 HNO3; G(B) = glass,
 borosilicate; G(S) = glass, rinsed with organic solvents or baked.
 ‡ g = grab; c = composite
 § Refrigerate = storage at 40C, in the dark.
 || Environmental Protection Agency, Rules and Regulations. 40 CFR Parts 100-149, July 1, 1992. See this citation for
 possible differences regarding container and preservation requirements.
 stat = no storage allowed; analyze immediately
 # If sample is chlorinated, see text for pretreatment.
Preparing Samples for Transport
• Verify that the number and type
of sample bottles match the Field
Data and Chain Of Custody Form
Site ID and Field Number
Date and Time of Collection
Sample Type and Preservation
 Preparing Samples for
Transport
DO’s DON’T’s
• Check that each bottle • Do not use tape or
is securely capped to paraffin on lids or jars
prevent leaking and containing organic
contamination samples

• Pack samples in fresh • Do not send samples

ice for shipping with a chilled with “blue Ice”
volume of ice equal to or other types of
at least the volume commercial, refreezable
occupied with samples containers.
DATA ANALYSIS
AND VALIDATION
DAO 90-35: Effluent Standards for Freshwater
CLASS
PARAMETER UNIT
AA A B C D
Temperature, max. 0C * 3 3 3 3
rise

pH Range * 6.0-9.0 6.0-9.0 6.5-9.0 6~9

Total Suspended mg/L * 50 50 70 150

Solids (TSS)

BOD5 @ 20 0C mg/L * 30 30 50 120

Oil & Grease (O/G) mg/L * 5.0 5.0 5.0 --

Total Coliforms (TC) MPN/100mL * 3,000 3,000 10,000 -

* discharge of effluent is not allowed

 References:

DENR EMB Effluent Quality

Manual Standard Methods
for Examination of Water
and Wastewater 22nd
Edition
end……