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DISINFECTION & CHLORINATION
PROCESS
OBJECTIVES
1. To be aware of the different disinfection methods.
2. To be aware of the proper chlorination process and its calculations.
DISINFECTION
➢ Process designed to kill or inactivate most microorganisms in wastewater, including
essentially all pathogenic organisms.

• UV Light
Physical
TYPES OF • Sterilization
DISINFECTION • Chlorination
METHODS Chemical • Copper Silver Ionization
• Ozonation
PHYSICAL DISINFECTION METHODS
Method Mechanism of Disinfection
Sterilization Sterilization is the process of killing all microorganisms. Sterilization also destroys
the spores of various organisms present on surfaces, in liquids, in medication, or in
compounds such as biological culture media. Categorized into: High
Temperature/Pressure Sterilization, Chemical Sterilization and Radiation
Sterilization.
UV Light Use of ultraviolet light or UV to disinfect or deactivate pathogens. This is
accomplished by exposing waterborne microorganisms to UV, having a wavelength
of 254 nm. The UV light damages the genetic materials of the organisms making it
incapable of continued growth or reproduction.
CHEMICAL DISINFECTION METHODS
Method Mechanism of Disinfection
Chlorination Use of chlorine or chlorine compounds which inactivates a microorganisms by deactivating its cell
membrane. Once the cell membrane is weakened, the chlorine can enter the cell and disrupt cell
respiration and DNA activity (two processes that are necessary for cell survival).
Ozonation Ozone has a greater disinfection effectiveness against bacteria and viruses compared to
chlorination. When ozone decomposes in water, the free radicals hydrogen peroxy (HO2 ) and
hydroxyl (OH) that are formed have great oxidizing capacity and play an active role in the
disinfection process. It is generally believed that the bacteria are destroyed because of
protoplasmic oxidation resulting in cell wall disintegration (cell lysis).
Copper-Silver Ionization Use the process of electrolysis.
Copper ions – destroys microorganisms cell wall and give way to silver ions to penetrate the core
of the microorganisms.
Silver ions – bonds to various parts of the cell, such as DNA and RNA, cellular proteins and
respiratory enzymes, causing immobilization, stop cellular growth and death of microorganisms.
Cupper Silver Ionization System

Ozonation System
UV Light Disinfection System
CHLORINATION
▪ A process of adding chlorine or chlorine compounds in wastewater such as sodium
hypochlorite and calcium hypochlorite.
▪ A method of adding chlorine intended for DISINFECTION and ELIMINATING
MICROORGANISMS such as bacteria and viruses in water.
CHLORINE CHEMISTRY
▪ Heavier than air
▪ Greenish-yellow colored
▪ Toxic gas
▪ One volume of liquid chlorine confined under pressure yields about 450 volumes
of gas.
▪ Strong oxidizing agent reacting with most elements and compounds.
▪ Moist chlorine is extremely corrosive.
▪ Vapor phase is a respiratory irritant.
CHLORINE IN WASTEWATER TREATMENT
▪ It acts as an oxidant.
▪ One of the most effective disinfectants.
▪ Known to deactivate or eliminate most pathogenic microorganisms.
▪ Easy to obtain
▪ Economical
▪ Easy to apply
▪ Effective
CHLORINE AND PATHOGENS
▪ Chlorine is most know to eliminate pathogenic microorganisms such as bacteria
and viruses, but ineffective to some microbes such as protozoa cysts.

Salmonella

Bacteria Virus Protozoa Cysts

Coliform
PATHOGENIC ILLNESSES

Pathogenic removal is important since the final discharge of effluent goes to the bodies of
water that serve as:

• Public water supplies


• Recreational uses
• Irrigation supplies
CHLORINATION SYSTEMS
▪ Elemental Chlorine (Chlorine gas)
❖ Use of greenish-yellow chlorine gas, cheaper and occupies less space
for storing; highly toxic and can cause chlorine gas explosions.
▪ Chlorine Solutions (Hypochlorites)
❖ Use of chlorine solutions such as Sodium Hypochlorite and Calcium
Hypochlorite.
▪ Chlorine Dioxide
❖ Cannot be stored and must be produced on site. Denatures protein in
bacteria and viruses even more effectively than chlorine.
REACTIONS OF CHLORINE
𝐶𝑙2 + 𝐻2 𝑂 → 𝐻𝐶𝑙 + 𝐻𝑂𝐶𝑙 𝐻 + + 𝑂𝐶𝑙−
𝑝𝐻>8

𝐶𝑙2 + 𝐻2 𝑂 → 𝐻𝐶𝑙 + 𝐻𝑂𝐶𝑙 𝐻+ + 𝑂𝐶𝑙−


𝑝𝐻<7

𝑂𝐶𝑙 −
CHLORINE GAS
❑ Highly oxidizing, toxic, corrosive and hazardous
yellow-green gas
❑ Can be lethal to human beings at 0.1% (volume)
concentration
❑ Requires specialized equipment, care and skill.
❑ Heavier than air and spreads slowly at ground level.
❑ Chlorine gas can be compressed to a point where its
liquifies. Cylinder contains both liquid chlorine (approx.
85%) and gas chlorine (approx. 15%)
❑ 100% available chlorine.
SODIUM HYPOCHLORITE (NAOCL)
▪ Acquired as liquid form either in carboys or bulk.
▪ Available in concentrations of 12.5%, 15 % and 7
%.
▪ General form of hypochlorite used in WWTPs.

2𝑁𝑎𝑂𝐶𝑙 + 2 𝐻2 𝑂 ⇒ 2 𝑁𝑎𝑂𝐻 + 𝐻𝑂𝐶𝑙 + 𝑂𝐶𝑙 − + 𝐻 +

𝑺𝒐𝒅𝒊𝒖𝒎 𝑯𝒚𝒑𝒐𝒄𝒉𝒍𝒐𝒓𝒊𝒕𝒆 + 𝑾𝒂𝒕𝒆𝒓 ⇒


𝑺𝒐𝒅𝒊𝒖𝒎 𝑯𝒚𝒅𝒓𝒐𝒙𝒊𝒅𝒆 + 𝑯𝒚𝒑𝒐𝒄𝒉𝒍𝒐𝒓𝒐𝒖𝒔 𝑨𝒄𝒊𝒅 + 𝑯𝒚𝒑𝒐𝒄𝒉𝒍𝒐𝒓𝒊𝒕𝒆 + 𝑯𝒚𝒅𝒓𝒐𝒈𝒆𝒏
CALCIUM HYPOCHLORITE (CA(OCL) ) 2

▪ Available in granules, pellets and powder.


▪ Also known as high test hypochlorite (HTH).
▪ Contains 65 – 70 % chlorine. The rest is
calcium.

𝐶𝑎(𝑂𝐶𝑙)2 + 2 𝐻2 𝑂 ⇒ 2 𝐶𝑎(𝑂𝐻)2 + 2𝐻𝑂𝐶𝑙


𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒚𝒑𝒐𝒄𝒉𝒍𝒐𝒓𝒊𝒕𝒆 + 𝑾𝒂𝒕𝒆𝒓 ⇒
𝑪𝒂𝒍𝒄𝒊𝒖𝒎 𝑯𝒚𝒅𝒓𝒐𝒙𝒊𝒅𝒆 + 𝑯𝒚𝒑𝒐𝒄𝒉𝒍𝒐𝒓𝒐𝒖𝒔 𝑨𝒄𝒊𝒅
CHLORINE DIOXIDE
▪ Relatively unstable chemical
▪ Manufactured at its point of use
▪ Result of reaction between chlorine gas/water
solution and sodium chlorite.

▪ Beneficial to use at pH above 8.5


CHLORINE REQUIREMENTS
Chlorine Dosage
▪ the amount of chlorine which must be added to produce a desired result
(i.e. disinfection of wastewater)

CHLORINE CHLORINE CHLORINE


DOSE DEMAND RESIDUAL

Chlorine Free
Combined Chlorine
CHLORINE REQUIREMENTS
Chlorine Demand
▪ The amount of chlorine used
by reactions with substances Organics ..can yield to
Chlororganics
that oxidize in the water Chlorine
before chlorine residual can Added/
be measured. Supplied
▪ May change with dosage, Inorganics
• Hydrogen Sulfide
• Ferrous Iron
time, temperature, pH, and • Manganese
the type and amount of • Nitrite
• Ammonia
pollutants in the water. (Chloroamines)
CHLORINE REQUIREMENTS
Residual Chlorine
▪ the chlorine in combined form (Chloroamines & Chlororganics) that have
disinfecting properties plus any free chlorine.
▪ The component of the applied chlorine that is available for disinfection.
• Chloroamines - a form of combined chlorine.
• Chlororganics - a weak form of combined chlorine.
• Free chlorine - the strongest form of residual for disinfection.
BREAKPOINT CHLORINATION

The point where chlorine


levels exceed the oxidant
demand, and the water
begins to build FAC (Free
Available Chlorine).
SAMPLE PROBLEM:
Given:
A wastewater is tested and found Chlorine Dose = 7.3 mg/L
to have a chlorine demand of 4.0 Chlorine Demand = 4.0 mg/L
mg/L and applied at 7.3 mg/L. If ChloroA = 1.7 mg/L
the desired chlorine residual is Free Chlorine = 0.8 mg/L
composed of 1.7 mg/L
chloroamines and 0.8 mg/L free Chlorine Dose = Chlorine Demand + Residual Chlorine
chlorine, what is the concentration Chlorine Dose = Chlorine Demand + ChloroA + Free Chlorine +
ChloroO
of the chlororganics in mg/L?
ChloroO = Chlorine Dose – Chlorine Demand – Chloro A – Free
Chlorine
ChloroO, mg/L = 7.3 mg/L – 4.0 mg/L – 1.7 mg/L – 0.8 mg/L
ChloroO, mg/L = 0.8 mg/L
CHLORINE DOSAGE
CHLORINE DOSAGE
𝒌𝒈 𝒎𝒈 𝒎𝒈 𝒎𝟑 𝒌𝒈
𝑭𝒆𝒆𝒅 𝑹𝒂𝒕𝒆 × 𝐏𝐮𝐫𝐢𝐭𝐲 = 𝐃𝐨𝐬𝐚𝐠𝐞 × 𝐅𝐥𝐨𝐰 × 𝟏𝟎𝟎𝟎 𝟑
FOR HTH: 𝒅𝒂𝒚 𝑳 𝑳 𝒅𝒂𝒚 𝒎

𝑃𝑢𝑟𝑖𝑡𝑦:

1% = 10,000 mg/L or ppm

FOR LIQ Cl: 𝑪𝒉𝒍𝒐𝒓𝒊𝒏𝒆 𝑺𝒕𝒐𝒄𝒌 𝑪𝒐𝒏′ 𝒏 × 𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑺𝒕𝒐𝒄𝒌 𝒕𝒐 𝒃𝒆 𝑫𝒐𝒔𝒆𝒅 = 𝑪𝒉𝒍𝒐𝒓𝒊𝒏𝒆 𝑫𝒐𝒔𝒂𝒈𝒆 × 𝑭𝒍𝒐𝒘
CHLORINE FEEDERS

Dry Feeder Gas Feeder


Solution (Liquid) Feeder
CHLORINATION PROCESS

Chlorinator

Decant from SBR

To Discharge Line
Effluent Pump
SAMPLE PROBLEM (DRY FEEDER):
𝒌𝒈 𝒎𝒈 𝒎𝒈 𝒎𝟑 𝒌𝒈
𝑭𝒆𝒆𝒅 𝑹𝒂𝒕𝒆 × 𝐏𝐮𝐫𝐢𝐭𝐲 = 𝐃𝐨𝐬𝐚𝐠𝐞 × 𝐅𝐥𝐨𝐰 × 𝟏𝟎𝟎𝟎 𝟑
An STP Operator, has been instructed by 𝒅𝒂𝒚 𝑳 𝑳 𝒅𝒂𝒚 𝒎

his supervisor to administer the chlorination


𝑚3
of the WWTP using HTH as a chlorite 𝐹𝑒𝑒𝑑 𝑅𝑎𝑡𝑒
𝑘𝑔
𝑑𝑎𝑦
× 650,000
𝑚𝑔
𝐿
=5
𝑚𝑔
𝐿
× 300
𝑑𝑎𝑦
𝑘𝑔
× 1000 3
𝑚
solution with 65 % chlorine purity fed
using a dry feeder. It has been the 𝑘𝑔 5 × 300 × 1,000
standard of the process to have an 𝐹𝑒𝑒𝑑 𝑅𝑎𝑡𝑒
𝑑𝑎𝑦
=
650,000
effluent chlorine dosage of 5 mg/L.
Having an average effluent flow rate of 𝒌𝒈 𝐤𝐠
𝑭𝒆𝒆𝒅 𝑹𝒂𝒕𝒆 = 𝟐. 𝟑𝟏
300 cubic meter per day, what is the feed 𝒅𝒂𝒚 𝐝𝐚𝐲

rate of the HTH?


SAMPLE PROBLEM
(WET FEEDER, HTH):
An STP Operator, has been instructed by his supervisor to administer the
chlorination of the treated wastewater using HTH as a chlorite solution with 70 %
chlorine purity fed using a chlorinator with 110 GPD as flow rate. It has been the
standard of the process to have an effluent chlorine dosage of 6 mg/L to comply
with coliform standards. The chlorinator runs simultaneously with the effluent with a
volume of 100 m3 per batch for about 90 mins. The powder chlorine is mixed in a
chlorine tank with a volume of 200L. (1) What is the volume and concentration (in
ppm) of the HTH solution that needs to be fed in the effluent tank? Using the
standard concentration of the HTH solution, (2) how many kg of HTH powder
needed in a 200L chlorine tank and (3) how many batches will it last? (4) If there
are 30 days in a month, how many kg of HTH is needed? The plant uses SBR
technology which has a standard 6 hr-process/batch.
SOLUTION:
Basis: 1. Determine the volume & standard
90 mins operation (1 batch) concentration of the HTH solution to be
70% HTH dosed in the effluent tank.
Chlorinator flow rate = 110 GPD ~
0.2892 lpm ~ 0.0002892 m3/min a. Volume of the chlorine fed in 90 mins
Effluent flow rate = 100 m3/batch
Chlorine tank volume = 200 L 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐶ℎ𝑙𝑜𝑟𝑖𝑛𝑒 𝑆𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝐹𝑒𝑑 = 𝐹𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝑇𝑖𝑚𝑒
Chlorine dose = 6 mg/L ~ 6 ppm 𝑚3
= 0.0002892 × 90 𝑚𝑖𝑛𝑠
𝑚𝑖𝑛

𝑽𝒐𝒍𝒖𝒎𝒆 𝒐𝒇 𝑪𝒍 𝒔𝒐𝒍′ 𝒏 = 𝟎. 𝟎𝟐𝟔𝟎𝟐𝟖 𝒎𝟑


SOLUTION:
b. Conc’n of the HTH Solution: 2. Kg of HTH needed to prepare HTH
𝐶𝑙𝑆𝑇𝐷 𝑉𝑆𝑇𝐷 = 𝐶𝑙𝐷𝑜𝑠𝑎𝑔𝑒 𝑉𝐷𝑒𝑐𝑎𝑛𝑡 solution in 200 L tank:
𝐶𝑙𝐷𝑜𝑠𝑎𝑔𝑒 𝑉𝐷𝑒𝑐𝑎𝑛𝑡 𝑘𝑔 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝐶𝑙𝑆𝑇𝐷 = 𝑝𝑝𝑚 = 𝑘𝑔 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
× 106
𝑉𝑆𝑇𝐷

(6𝑝𝑝𝑚)(100𝑚3 ) 𝑘𝑔 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝐶𝑙 = 𝑘𝑔 𝑜𝑓 𝐻𝑇𝐻 (% 𝑃𝑢𝑟𝑖𝑡𝑦)


𝐶𝑙𝑆𝑇𝐷 = 0.026028 𝑚3
𝑘𝑔 𝑜𝑓 𝐻𝑇𝐻 (70%)
𝑪𝒍𝑺𝑻𝑫 = 𝟐𝟑, 𝟎𝟓𝟐. 𝟎𝟗𝟕𝟕 𝒑𝒑𝒎 23,052.0977 𝑝𝑝𝑚 = × 106
𝑘𝑔
200 𝐿 (1 )
𝐿
𝒌𝒈 𝒐𝒇 𝑯𝑻𝑯 = 𝟔. 𝟓𝟖𝟔 𝒌𝒈
SOLUTION:
3. No. of batches that the chlorine 4. Monthly Requirement:
contents in a tank (full capacity) will last.
6.586 𝑘𝑔 1 𝑡𝑎𝑛𝑘 4 𝑏𝑎𝑡𝑐ℎ𝑒𝑠
𝐾𝑔, 𝑚𝑜𝑛𝑡ℎ𝑙𝑦 = ( )( )( )(30 𝑑𝑎𝑦𝑠)
1 𝑡𝑎𝑛𝑘 7 𝑏𝑎𝑡𝑐ℎ𝑒𝑠 1 𝑑𝑎𝑦
𝑉𝑐ℎ𝑙𝑜𝑟𝑖𝑛𝑒 𝑡𝑎𝑛𝑘
𝑁𝑜. 𝑜𝑓 𝑏𝑎𝑡𝑐ℎ𝑒𝑠 = 𝑉𝑑𝑜𝑠𝑒𝑑/𝑏𝑎𝑡𝑐ℎ
𝒌𝒈, 𝒎𝒐𝒏𝒕𝒉𝒍𝒚 = 𝟏𝟏𝟐. 𝟗 𝒌𝒈
200 𝐿
=
1000 𝐿
(0.026028 𝑚3 )( )
1 𝑚3 if 1 drum of HTH = 40 kg, how
many drums of HTH is needed?
𝑵𝒐. 𝒐𝒇 𝒃𝒂𝒕𝒄𝒉𝒆𝒔 = 𝟕. 𝟔𝟖 ~ 𝟕
𝒅𝒓𝒖𝒎 𝒐𝒇 𝑯𝑻𝑯 = 𝟐. 𝟖 ~ 𝟑
SAMPLE PROBLEM
(WET FEEDER, SODIUM HYPOCHLORITE):
An STP Operator, has been instructed by his supervisor to administer the
chlorination of the treated wastewater using sodium hypochlorite solution with 7 %
chlorine purity fed using a chlorinator with 110 GPD as flow rate. It has been the
standard of the process to have an effluent chlorine dosage of 6 mg/L to comply
with coliform standards. The chlorinator runs simultaneously with the effluent with a
volume of 100 m3 per batch for about 90 mins. The powder chlorine is mixed in a
chlorine tank with a volume of 200L. (1) What is the volume and concentration (in
ppm) of the chlorine solution that needs to be fed in the effluent tank? Using the
standard concentration of the chlorine solution in No. 1, (2) how many liters of the
7% Sodium Hypochlorite solution is needed in a 200L chlorine tank and (3) how
many batches will it last? (4) If there are 30 days in a month, how many L of HTH is
needed? The plant uses SBR technology which has a standard 6 hr-process/batch.
FACTORS INFLUENCING DISINFECTION
▪ Proper point of injection and thorough mixing.
▪ Contact Time
✓ 15 mins at peak hourly rate
✓ 30 mins at maximum month average flow
▪ Effective pretreatment (lower TSS/organics will allow disinfection to be more effective)
▪ Lower pH will result in more efficient chlorination
▪ Higher Temperature will result in more efficient disinfection.
▪ Higher dosages of disinfectant will in more rapid disinfection.
▪ Longer detention time will result in higher degree of disinfection.
DANGERS OF CHLORINE
▪ Highly toxic and corrosive chemical.
▪ An oxidant and disinfectant.
▪ Its gas form acts as an irritant for respiratory and other mucous
membranes.
▪ Its liquid form can burn skin.
▪ Humans can smell as low as 3.5 ppm.
▪ Few breaths at a concentration of 1000 ppm is usually fatal.
BREAK 15 MINS….
STANDARD SAMPLING PROCEDURES
OBJECTIVES
1. To gain knowledge and understanding on the type of samples and how to conduct
proper sampling
2. To gain knowledge on the required materials and the quality assurance in
conducting proper sampling.
3. To know the effect of mishandling the samples in the laboratory results.
4. To know the standard protocols during regulatory sampling.
REFERENCES ON THE CONDUCT OF SAMPLING:
▪ Water Quality Monitoring Manual Volumes I & II of DENR – EMB
▪ Work Instruction of Process O&M (ECO-WI-POM-01 STP Influent & Effluent
Sampling)
▪ Wastewater Operator Certification Training, Module 12: Laboratory Overview
SAFETY ON SAMPLING
▪ Always follow rules and regulation in WWTP.
▪ Do not touch motors and air pipelines.
▪ Do not smoke or eat during sampling.
▪ Wear appropriate personal protective equipment such as hard hat, gloves,
goggles.
▪ When using gloves we are protecting the sample and the sample collector.
▪ Always wash hands with soap and water or disinfect with 70% alcohol after
sampling.
LABORATORY HYGIENE & SAFETY
Laboratory Hygiene
❑ refers to the process in which plant operator employs safe practices when
handling known or suspected hazardous material.
❑ minimize the opportunity for exposure to infectious or toxic substances
(chlorine solution).
Must consider in handling:
▪ be aware of the information of the chemical hazard through its MSDS.
▪ use PPE when handling chemicals and wastewater.
▪ observe personal hygiene.
ROUTES OF INFECTION IN HANDLING OF
CHEMICALS OR WASTEWATER:
▪ Cutaneous
❑ route for most bacterial infections; wash hand on frequent basis; wear
gloves or cover breaks in skin.
▪ Oral Ingestion
❑ route for viral and some bacterial infections; thorough hand washing
and immunization against viral pathogens; consider changing out of
work clothes before returning home; work and street clothes should
be stored in separate lockers.
▪ Inhalation
❑ route for most airborne disease transmission; best defense is
immunization and personal hygiene; wear protective masks.
EFFLUENT QUALITY MONITORING
Effluent
❑ defined by PCWA, discharges from unknown source which are passed into a
body of water or land or wastewater flowing out of a manufacturing plant, or
industrial plant including domestic, industrial or recreational facilities.

Effluent Quality Monitoring


❑ process of checking, evaluating or investigating the quality of the effluent or
wastewater discharges from an industry, establishment or facility.
OBJECTIVES OF EFFLUENT QUALITY MONITORING
▪ Ensure compliance to GES (within allowable concentration limits).
▪ Basis for regulatory and control actions (issuance of DP, NOV, CDO)
▪ Evaluate the effectiveness of effluent treatment and control
▪ Identify potential environmental problems and recommend mitigating measures
▪ Determine the impact to the receiving media (water body, groundwater and land)
▪ Support permit revision and/or renewal based on new data
▪ Detect, characterize and report unplanned releases by the facility
▪ Determine the effectiveness of the waste minimization/cleaner technologies adopted by
the facility.
SAMPLING
Definition
▪ taking a representative portion of the materials
small enough to be transported to the laboratory
but large enough for the parameters to be
tested.
Importance
▪ In order to analyze a sample it must be collected.
▪ Collect a sample that is truly a representative of
the conditions that exists at the time of collection
PURPOSE OF SAMPLING
Planning

Research

Process Control

Regulation
TYPE OF SAMPLES
Grab Sample
▪ also called as catch, spot or snap sample.
▪ one sample is taken at a time and at given location.
▪ only characterize the waste at the time collected and does not represent the
average conditions.
▪ neither flow nor time based; can be collected at any time and at any flow.
TYPE OF SAMPLES
Grab Sample
Suitable when:
❖ analyzing situations at specific site
❖ analyzing for unstable parameters that have to be measured right away
or on site (DO, temperature, pH, TDS, salinity)
❖ a snapshot of water quality at a particular instant is desired
❖ the characteristics of the waters are known to be relatively constant over
time.
❖ collecting samples to be analyzed for parameters that could be adversely
affected by compositing process.
TYPE OF SAMPLES
Composite Sample
▪ series of individual grab samples taken at different times from the same
sampling point and mixed together, PNSDW of 2007.
▪ may also be a number of grab samples of equal or weighted volumes mixed in
one container.
▪ more accurately characterizes the average quality of the wastewater.
▪ preferred when the concentration of the parameter under consideration is
expected to vary with time (or location)
TYPE OF SAMPLES
Type of Composite Sample:
▪ Fixed Volume Composite Sample
Time & size sample remains constant; used when the average flow rate of the
wastewater does not vary more than the 15% of the average flow.
▪ Time Composite Sample
Mixing samples of equal volume collected at regular time interval.
TYPE OF SAMPLES
Type of Composite Sample:
▪ Flow-proportioned Composite Sample
❖ Fix flow – volume remains the same and the time interval between sampling
varies; taking 1 L for every 100 m3 of flow.
❖ Variable flow – as flow increases sample taken increases
▪ Depth-integrated Composite Sample
Collected in pre-determined depths of the water column in equal water
volumes and mixed in one container.
COMPOSITE SAMPLING
▪ Collect individual samples based on schedule.
▪ Determine flowrate at the time of sampling.
▪ Calculate specific amount to add to the container.
𝑉𝑜𝑙𝑢𝑚𝑒 𝑡𝑜 𝑏𝑒 𝑎𝑑𝑑𝑒𝑑 = 𝐹𝑙𝑜𝑤 × 𝑃𝐹
𝑃𝑟𝑜𝑝𝑜𝑟𝑡𝑖𝑜𝑛𝑖𝑛𝑔 𝐹𝑎𝑐𝑡𝑜𝑟 = (𝑟𝑜𝑢𝑛𝑑 𝑜𝑓𝑓 𝑡𝑜 𝑡ℎ𝑒 𝑛𝑒𝑎𝑟𝑒𝑠𝑡 0.5 𝑢𝑛𝑖𝑡𝑠))
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑
𝑃𝐹 =
𝑁𝑜. 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒𝑠 𝑡𝑜 𝑏𝑒 𝑐𝑜𝑙𝑙𝑒𝑐𝑡𝑒𝑑 × 𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑎𝑖𝑙𝑦 𝐹𝑙𝑜𝑤
▪ Mix the individual sample thoroughly .
▪ Measure the required volume and add it to the composite container.
▪ Refrigerate the composite sample throughout the sampling.
SAMPLE PROBLEM
You need to run samples for GES compliance but the effluent autosampler is broken. Your
supervisor told the operators to get grab samples, put them in the refrigerator and to read the
effluent totalizer every two hours. This morning he has told you to take the individual grab
samples the operators collected and make the composite sample yourself. You are required to
do a flow based composite and you will need about 1,000 mL of the sample to conduct all the
required test. The night shift operator provides a summary of the data as follows:
Compute for the Proportion Factor and Required Volume of sample per time interval.
Time Flow Time Flow Time Flow
Reading Reading Reading
12 mn 0 10 am 150 8 pm 453
2 am 17 12 nn 186 10 pm 615
4 am 35 2 pm 230 12 mn 785
6 am 68 4 pm 340
8 am 102 6 pm 389
SOLUTION
No. of samples required = 12
Total volume of sample needed = 1,000 mL

785 𝑚3
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐹𝑙𝑜𝑤 = = 65.41667 𝑚3
12

𝑇𝑜𝑡𝑎𝑙 𝑉 𝑜𝑓 𝑆𝑎𝑚𝑝𝑙𝑒 1000 𝑚𝐿


𝑃𝑟𝑜𝑝𝑜𝑟𝑡𝑖𝑜𝑛 𝐹𝑎𝑐𝑡𝑜𝑟 = 𝑁𝑜.𝑜𝑓 𝑆𝑎𝑚𝑝𝑙𝑒 ×𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐹𝑙𝑜𝑤 = 12 ×65.41667
= 𝟏. 𝟐𝟕𝟒
SOLUTION
Vol. of
Time Flow Reading Flow PF
Sample, mL
12:00 AM 0
2:00 AM 17 17 1.274 22
4:00 AM 35 18 1.274 23
6:00 AM 68 33 1.274 42
8:00 AM 102 34 1.274 43
10:00 AM 150 48 1.274 61
12:00 PM 186 36 1.274 46
2:00 PM 230 44 1.274 56
4:00 PM 340 110 1.274 140
6:00 PM 389 49 1.274 62
8:00 PM 453 64 1.274 82
10:00 PM 615 162 1.274 206
12:00 AM 785 170 1.274 217
Total Volume of Sample 1000
ACTIVITIES IN STP WHERE SAMPLING IS
OBSERVED:
❑ Influent Sampling
❑ Effluent Sampling
❑ Sludge settleability Test
IN ORDER TO MEET THE GOALS OF EFFLUENT
SAMPLING, THE DATA COLLECTED MUST BE..
❑ Representative
❑ Reproducible
❑ Defensible
❑ Useful
GENERAL CONSIDERATIONS IN SAMPLING
❑ Location of Establishment, Type of Industry, Type of WTP
❑ Number and location of the discharge outlet and permit condition
❑ Number of samples and parameters to be analyzed
❑ Sampling containers, devices and field tests to be performed
❑ Sampling procedures
❑ Labelling
❑ Preservation and Transport
❑ Traceability of sample
❑ Documentation
LOCATION OF ESTABLISHMENT, TYPE OF
INDUSTRY & TYPE OF WWTP
▪ This information is reflected in
the Discharge Permit of the
establishment.
LOCATION OF ESTABLISHMENT, TYPE OF
INDUSTRY & TYPE OF WWTP
▪ This information is reflected in
the Discharge Permit of the
establishment.
LOCATION OF SAMPLING
Check the sampling point where to collect and see if it is safe to collect sample. Do not
enter manhole or confine space/ without necessary permit from authority/ supervisors.
General considerations:


LOCATION OF SAMPLING
WQMM Volume II Section 3.4 Selection of Sampling Stations:
LOCATION OF SAMPLING
Correct Sampling Points in the STP:
❑ Discharge Pipe (Must be on the center of
flow and after chlorination)
❑ Sampling ports (Taps)
NUMBER OF SAMPLES & PARAMETERS TO BE
ANALYZED
SAMPLING DEVICES
▪ Bucket or Jar
▪ Bottles
▪ Depth Sampler
▪ Sludge Sampler
▪ Composite Auto Samplers
SAMPLING BOTTLES/CONTAINERS
SAMPLING BOTTLES
General Considerations:
▪ Ensure enough containers to hold the samples for specific parameters.
▪ Inspect all containers for damages (cracks and chips) and for cleanliness. Do not use
containers with visible defects or discoloration.
▪ Do not use containers that have been used for storage of chemicals or other liquids. All
containers must be decontaminated according to recommending procedure.
▪ The analyses to be performed on the sample dictate the type of sample containers.
▪ For microbiological analysis, strong, thick-walled glass sample bottles with a minimum
capacity of 120 mL are recommended. The bottles should have screw caps of a type that
will maintain an effective seal even after having been autoclaved many times.
SAMPLING BOTTLES
Cleaning of Sample Containers:

Table 6.1 Sample Containers for


Specific Water Quality Parameters
and recommended cleaning
procedures
Water Quality Monitoring Manual
Volume II, DENR-EMB
TESTING KITS AND INSTRUMENTS
PRE - SAMPLING PROCEDURES
1. Must have information prior to sampling:
❖ Type of Analysis
❖ Type of Sample
❖ Volume Required (coordinate with the Laboratories)
Ex: Grab Sampling, BOD Analysis, 1 L
PRE - SAMPLING PROCEDURES
2. Prepare the resources needed for sampling.
❖ Personal Protective Equipment (PPEs) – gloves (a must), goggles, mask, hard
hat and safety shoes (if applicable).
❖ Hand soap or 70% alcohol for sanitation.
❖ Chlorine solution for disinfecting pail, dippers, samplers, discharge pipe
opening, tap or faucet opening.
❖ Pail and dipper for split sampling
❖ Secondary sampler/depth sampler (improvised depth sampler)
PRE - SAMPLING PROCEDURES
2. Prepare the resources needed for sampling.
❖ Sampling bottles (if not in use, store in a clean area, free from oil, dust and
chemicals)
➢ Plastic Gallon (at least 4 Liters) – for general parameters such as
BOD, COD, TSS and Color.
➢ Wide mouth glass bottle with aluminum lined cap (at least 1 Liter) –
for Oil and grease parameter.
➢ 250/ 500 mL PET bottle or Whirl pack plastic (at least 100 mL) –
for coliform parameter.
PRE - SAMPLING PROCEDURES
2. Prepare the resources needed for sampling.
❖ For sample preservation: prepare ice box, ice and zip locks.
❖ For sample labelling: permanent market, pen, masking tape, paper
❖ For documentation: camera or smartphone.
❖ If chemicals are needed for preservation, observe proper handling and
storage of the chemicals based on its Materials Safety Data Sheet.
PRE - SAMPLING PROCEDURES
3. Check the sampling point or location.
❖ Sampling point must be safe and accessible.
❖ Do not enter manhole/confined spaces without necessary permit from
authority/supervisors.
❖ The operator must sanitize the discharge pipe opening (if accessible), tap
or faucet by wiping a cloth with chlorine solution before the sampling
activity.
PRE - SAMPLING PROCEDURES
4. Wear appropriate PPEs.
❖ Use gloves to protect you and the sample.
❖ Use hard hat for areas with overhead pipelines
❖ Use mask for handling chemicals and fumes
PRE - SAMPLING PROCEDURES
5. Pre-label bottles and containers with the following information:

Sample Identification No. (if applicable)


Project Name Citynet STP
Type of Sample Wastewater: Effluent
Date of Collection April 21, 2021
Time Collected 8:30 AM
Name of Collector Juan dela Cruz
On-site Analysis pH – 8.2

Wrap with clear tape on top of the sticker label to make sure
that it is intact upon receipt in the laboratory.
PRE - SAMPLING PROCEDURES
Thing to remember prior to sample collection:
❑ Check ID of sampler and record in logbook.
❑ Must have enough chlorine dosage and chlorine contact time of at least 30 mins.
❑ Keep all resources aware from areas with oil spill, dust, and mist as this will
contaminate the sampling bottles, as well as the samples. Put it in the cleanest area
in the STP when stored and during sampling.
DURING SAMPLING PROCEDURES
A. Direct Sampling with Sample Container
➢ Put on protective gloves and other necessary PPEs.
➢ Open the tap and flush lines to remove stagnant water along the line,
do the same when collecting sample in decant or discharge pipes.
When sampling on tap, lower the flowrate approximately to 0.5 gpm
and collect the sample.
➢ Obtain a pre-labeled sample bottle or container and remove the lid
without touching the inner surface of either the bottle or the lid.
➢ Rinse the container at least three times with the effluent, except for
container with preservative and for sample intended for Oil and
Grease, and coliform parameter.
Sampling port (Tap)
CGC
DURING SAMPLING PROCEDURES
A. Direct Sampling with Sample Container
➢ Hold the bottle below the neck and lower it into the effluent. Ensure that the hands do
not touch the bottle opening.
➢ For FOG bottles, take samples only from the surface of the water. Do not submerge
the sample bottle below the water surface.
➢ Slowly lift the container towards the flow. Fill it to about 4/5 full. Enough space should
be left to allow for the addition of preservative, if necessary, and to allow for mixing
the sample.
DURING SAMPLING PROCEDURES

**Water Quality Monitoring Manual, Volume II


DURING SAMPLING PROCEDURES
B. Sampling with Intermediate Container
▪ Intermediate container (bucker, dipper, & samplers) to collect grab sample is
employed for the following conditions:
✓ If sample cannot be obtained by direct sampling (deep tanks, wastewater
ponds).
✓ If volume/flowrate of effluent discharge is high.
✓ If there is a need to do split sampling.
DURING SAMPLING PROCEDURES
B. Sampling with Intermediate Container
When using samplers:
➢ Samples can be obtained at distances as far as 3 m
from the edges of the source, preventing the sampler
from having contact the source physically.
➢ Must be decontaminated prior use.
➢ Can either be reused or discarded.
DURING SAMPLING PROCEDURES
B. Sampling with Intermediate Container
When using bucket:
➢ Must be decontaminated prior use.
➢ Sampling bottle must be clean outside and must be held
at an angle and submerged into the liquid until it is full
and air bubbles have been expelled at which time it is
carefully retrieved, preserved as necessary and capped.
➢ Avoid sample contamination from the outer part of the
sampling bottles or containers.
➢ During split sampling, use a dipper to collect sample and
transfer it equally to the receiving sampling bottles.
DURING SAMPLING PROCEDURES

**Water Quality Monitoring Manual, Volume II


DURING SAMPLING PROCEDURES
For BOD Parameter:
▪ Use either BOD bottle or plastic gallon.
▪ Over flow the bottles and ensure there is no bubbles entrap.
▪ Cap the bottles, seal with tape (tampered seal) and make sure
that there is no leak.
▪ Ensure that the sample has label.
▪ The bottle can be sealed in a zip lock and must be contained in an
ice box for preservation and transport.
DURING SAMPLING PROCEDURES
For Oil and Grease Parameter:
▪ Use wide mouth glass bottles with aluminium foil lining or
Teflon lining.
▪ After flushing the line, Collect the sample directly from
sampling point to glass bottle ( do not rinse the bottle)
▪ Do not overfill the sample. Fill only up to ¾ of the bottle.
▪ Cover the bottle with a cap lined with aluminium foil or use
teflon lined cap
▪ Ensure there is no leak.
▪ Ensure sample has label.
DURING SAMPLING PROCEDURES
For Microbiological Paramater (Coliform):
▪ Ensure that the sample is properly chlorinated and with enough contact time.
When using coliform glass/PET bottle:
➢ Use glass bottle with cap line with aluminum foil. Clean and non-contaminated
PET bottle can be used as an alternative.
➢ Do not wash the bottle with sample. Fill the sample bottle with sample up to
¾ of the sample container.
➢ Cap the sample bottle and ensure no leakage. Record the time of sampling.
DURING SAMPLING PROCEDURES
For Microbiological Paramater (Coliform):
▪ Ensure that the sample is properly chlorinated and with
enough contact time.
When using Whirl Pack:
➢ Label the whirl pack.
➢ After flushing line, tare the upper portion of the
whirlpack and pull the tabs.
➢ Collect sample directly to the whirlpack.
➢ If using secondary sampler ensure that it is clean and
wash with Chlorine and dry.
➢ Turn the Whirlpack to seal and bend the end wire.
DURING SAMPLING PROCEDURES
DURING SAMPLING PROCEDURES
On-site Measurement:
▪ Obtain actual values of on-site parameters using instruments such as pH
meter, temperature probe meters, residual chlorine meter, etc.
▪ This is necessary since effluent quality might change during transport to the
laboratory.
POST SAMPLING PROCEDURES
(PRESERVATION, STORAGE & TRANSPORT)
❑ Rinse the outside surface of the sample contained with tap water before
placing inside the cooler or ice chest to prevent contamination.
❑ Transport the sample immediately to the Laboratory.
❑ If transportation will be more than 1 hour, put the sample containers in a
cool box with crushed, tube ice or icepack to preserve the sample to 4 –
6 ℃.
❑ Samples may be stored in dark to retard biological activity and reduce
the change in physical and chemical properties of water samples.
❑ Separate the glass bottle to one another to avoid breakage.
POST SAMPLING PROCEDURES
(PRESERVATION, STORAGE & TRANSPORT)
❑ If other parameters are required, refer to sample preservation required
as per Standard Method for the Examination of Water and
Wastewater.
❑ Fill up necessary information in the laboratory endorsement form or
chain of custody.
❑ Wash hands with soap and water or with 70% alcohol for disinfection.
❑ Clean the area.
POST SAMPLING PROCEDURES
(PRESERVATION, STORAGE & TRANSPORT)
CHAIN OF CUSTODY
❑ This is a record to show the traceability of sample from the time of
sampling until the sample reception in the laboratory. This also include
the temperature of sample upon receipt of the laboratory.
❑ Chain of custody can be used in the court.
DOCUMENTATION
According to the WQMM VII, “Documentation must be available to validate the sampling
procedures. The data must have known degree of accuracy and precision”.
Table 6.2 (Checklist for Preparatory Activities, Materials, Equipment and Supplies)
3. For Documentation
✓ Pens & clipboard
✓ Sample labels
✓ Logbook or field notebook
✓ Camera or recorder for photo documentation
REGULATORY SAMPLING PROTOCOLS
❑ Upon arrival of regulatory representatives, greet them with utmost respect.
❑ Check if they are accompanied by the client’s PCO or representative.
❑ Upon arrival of the regulatory and client representative, check for the
following politely:
✓ Official Vehicle with Logo
✓ Identification Card (Valid ID)
✓ Mission order
✓ PPEs necessary for sampling
REGULATORY SAMPLING PROTOCOLS
❑ If the regulatory representative does not have gloves, offer them one for their
usage during the sampling activity.
❑ Orient the regulatory of the safety protocols in the STP. Do not allow persons
wearing slippers inside the STP.
❑ Ask the regulatory representative/s on what parameters will be tested.
❑ Observe proper sampling procedures as discussed in the previous slides.
❑ The DENR/LLDA representative must be the one to get and collect the
sample.
REGULATORY SAMPLING PROTOCOLS
❑ Observe proper procedure in the conduct of split sampling.
❑ When sampling is done, record the details on the STP logbook:
• Date of Sampling
• Time of Sampling
• Time of Decant
• Parameters to be tested
• On-site parameter measured (Such as pH)
• Name of DENR/LLDA Representative (signed by them)
REGULATORY SAMPLING PROTOCOLS
❑ Inform and politely request the samples of the regulatory to be contained in an
ice box (with enough ice) provided by ESTII. Make sure that the bottles are
properly sealed (stored in zip locks) and labeled.
❑ Add enough ice to ensure that the temperature inside the ice box must be
around 4-6 deg. C.
❑ Seal the box with a tape, label properly and have it signed by the client’s
PCO.
❑ Take documentation of the sampling activity.
❑ Deliver the split samples immediately to the laboratory upon departure of the
regulatory.
WAYS TO PREVENT CONTAMINATION ON THE
EFFLUENT
❑ Observe cleanliness of the contact tank.
▪ Daily – Drained
▪ Monthly/Quarterly – General Cleaning
❑ Apply shock dosing of chlorine (20 ppm) to clean discharge pipes at least once a
month.
❑ If its not feasible to drain the tank due to the existing installation of the pump (no
sump pit), chlorine dosage must be increased. Chlorine must be dosed to the tank
daily with or without decant.
EPA WATER SAMPLING PROCEDURES
https://www.youtube.com/watch?v=exyVfFIn7TQ
END.

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