Sampling and Field Testing at Wastewater Facilities Presented by Jenny Farrell and Debra Knight

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Sampling and Field Testing at Wastewater
FacilitiesPresented by Jenny Farrell and Debra
Knight
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Overview

• Where to find the FDEP rules about field sample
  collection
• Sampling procedures
• Field testing and meter calibration
• QA Plans for Field Procedures
• New Draft QA Rule and SOPs

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Where to find the Rules

• Wastewater Permit, Part I, Monitoring
• F.A.C. 62-625 Wastewater Monitoring Rule
• F.A.C. 62-160 Quality Assurance Rule
• Field DEP SOP - 001/01 revised on February 1,
  2004
• http//www.dep.state.fl.us/labs/qa/sops.htm
• http//www.epa.gov/region4/sesd/eisopqam/eisopqam.
  pdf

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Which SOPs do I need????

• DEP SOP - FD 1000 Documentation
• DEP SOPs / Sampling
• FC 1000 Field Decontamination
• FQ 1000 Quality Control
• FS 1000 General Sampling
• FS 2000 General Water Sampling
• FS 2400 Wastewater Sampling
• DEP SOPs / Testing
• FT 1000 Field Testing General
• FT 1100 Field pH
• FT 1600 Field Turbidity
• FT 1800 Field Flow Meters
• FT 1900 Field Continuous Monitoring
• FT 2000 Field Residual Chlorine
• other

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Sampling Points

• As described in the permit
• influent (in most cases prior to any plant
  process recycled water)
• CBOD5, TSS
• effluent after filtration before disinfection
• continuous turbidity or TSS and grab TSS for
  high level disinfection
• effluent after chlorination
• most sampling, including CBOD5, TSS, nutrients,
  TRC (check if 15 minutes retention time is
  assured), and other per permit requirements
• residuals
• Class B
• Class A/AA

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Sampling Types

• Grab samples
• grab directly into a sample container or with
  intermediate vessel like dipper or bucket
• submerge container neck first
• invert bottle so the neck is upright pointing
  into the water flow
• add preservative, cap container and label
• FC, VOC, un-ionized ammonia are always grab
  samples
• Time composite samples (seldom required)
• Flow- proportioned composite samples
• automatic sampler and associated flow measuring
  device
• manually , size of the aliquot determined with a
  flow chart
• collect a minimum of 100 mL for each aliquot

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Sampling Containers

• DEP SOP Table FS 1000-4 and 40 CFR Part 136 Table
  II
• Nutrients, CBOD, TSS plastic or glass
• Coliforms plastic or glass, sterile
• Turbidity plastic or glass
• Metals usually plastic, glass is accepted except
  for boron, chromium IV, and mercury
• Oil grease glass, wide mouth
• Organics glass with teflon lined cap

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How to collect a representative sample

• Center of the flow where velocity is highest
• 40-60 of the total depth (except FC)
• if collecting from a sample tap allow the sample
  to run for one to two minutes

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Sampling Equipment

• Select sampling equipment
• buckets, spatulas, dippers, tubing, etc.
• Table FS 1000-1 and FS 1000-2

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Sampling Equipment, cont.

• Composite samplers
• must be able to maintain temperature between 1 to
  4oC2oC
• must be properly maintained and cleaned
• intake line must be purged before each sample
  aliquot is collected
• individual sample aliquot must be at least 100 mL
• adequate power source should be available to
  operate the samples. Remember often samplers
  have their own battery source that needs to be
  changed or recharged before events.

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Tips about automatic samplers

• Typically samplers should be located as close to
  the sampling point as possible both in elevation
  and in distance. Maximum heights between water
  surface elevation should not exceed 20 feet in
  most cases.
• Sample lines should be set up so that there are
  no sags or dips in the line that would prevent
  the line from draining when not in use.
• Access to equipment should be limited to prevent
  vandalism, yet provide personnel ample room to
  remove heavy sample bottles and replenish ice, if
  used.

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Tips about automatic samplers Before starting
the sampler

• Check all electrical connections for tightness.
• Check the sampler humidity indicator located on
  the control panel. If it is PINK it is time to
  change out the de-humidifying crystals
  (electronic circuit boards may fail in a moist
  environment).
• Check the intake tubing for kinks or twists and
  clamps for tightness and condition. Check the
  pump tubing for cracks and working out any
  pinches or replace if needed.
• Understand how to program the sampler in case the
  program get wiped. Also settings may need to be
  adjusted if the plant flow changes or if the auto
  sampler has to be moved

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Bacteria Sampling

• microbiological samples, if possible, collect
  sample directly into a sterile sampling
  container
• do not rinse sample container with
• the sample water
• when using intermediate sampling equipment,
• clean it thoroughly and rinse several
• times with sample water before collection
• intermediate sampling equipment
• does not require sterilization

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Sample Preservation

• Follow table 4 in SOP FS 1000 for required
  containers, preservation techniques, and holding
  times
• Generally, preserve samples (FS 1000.FS 1006
  (5))
• within 15 minutes from sample collection
• cool to 4oC by placing it on ice
• Add preservative/treatment
• Na2S2O3 for fecal coliforms to dechlorinate
  sample
• Any preservation, including thermal must be
  recorded on the COC.
• Receiving laboratory is required to check.
• They should contact you if not indicated on COC.
• Sample results will be qualified

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Sample Collection, Reuse Pathogenic Monitoring

• Giardia and Cryptosporidium, EPA Method 1623
• sample may be filtered in the field or in the
  laboratory
• preserve samples by cooling to 0-8oC (do not
  freeze)
• start analysis ASAP, no later than 96 hours after
  collection
• Special DEP Requirements
• see Instructions to DEP Form 62-610.300(4)(a)4.,
  March 9, 2006
• report due to DEP on or before November 28 of
  each even year or at permit renewal
• detection limit of 5 Giardia cysts and 5
  Cryptosporidium oocysts per 100 L has to be met
• samples shall be recollected every 90 days if
• number of potentially viable cyst of Giardia
  exceeds 5/100 L
• number of potentially viable oocysts of
  Cryptosporidium exceeds 22/100 L

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Residuals Sample Collection

• EPA Control of Pathogens and Vector Attraction
  in Sewage Sludge (White House Manual)
  http//www.epa.gov/ORD/NRMRL/Pubs/1999/625R92013.p
  df
• Table 6 DEP SOP FS1000
• Collect representative sample
• Grab - liquid and well mixed samples
• Composite - thick or dry residuals
• Fecal coliform (FC) holding time is 24 hours
• Sample preservation - place on ice or
  refrigerate no acid
• Class A/AA
• FC cannot exceed 1000 fc/1 gram dry weight
• Class B
• FC geometric mean of seven grab samples
  collected over at least two week period

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Sampling Records

• Use waterproof ink for all paper documentation
• Make corrections by marking a line through the
  error so that it is still legible. Initial or
  sign the marked error
• Date and time of sample collection for composite
  samples document date and time of first and last
  aliquot
• Name of the person collecting sample
• Description of sampling site (e.g. effluent from
  CCC)
• Site address
• Field ID number for each container
• Number of containers
• Analyses required
• Preservative used

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Field Testing and Certification

• No certification by the DOH ELCP is required when
  conducting the following test procedures
• pH
• Dissolved oxygen
• Specific conductivity
• Temperature
• Total residual chlorine (including free available
  chlorine)
• Turbidity (when performed at the sampling
  location)
• Sediment oxygen demand
• Any other test with a specific holding time of
  fifteen minutes or less when performed at the
  sampling location
• Any analyses related solely to internal process
  control
• All results have to be reported to the Department
  for samples collected at compliance locations and
  performed in accordance with the DEP SOPs

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Field Measurements - pH

• pH meter requirements
• meter consisting of potentiometer, glass
  electrode, reference electrode, and temperature
  compensating device
• low sodium electrode should be used for samples
  at pH ? 10.0 (Biosolids)
• accurate and reproducible to at least 0.2 unit in
  the range of 0.0 to 14.0 units
• calibration
• calibrated with at least two pH buffers.
• always use pH buffer 7.0 first
• buffers must bracket the expected sample pH
• second buffer must be at least three pH units
• apart (4.0. or 10.0)
• if third calibration point needed and instrument
  cannot be calibrated with three buffers, use the
  third buffer as a calibration check

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Measuring pH

• Rinse the probe with DI water
• Pour out sample or place probe in the effluent
• Stir the sample!
• When you have a stable reading
• Record it !
• (If you dont write it down you havent done it)

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Field Measurements - pH cont.

• pH continuous meters
• initial calibration
• before installation and
• each time the instrument is taken off-line
• after fails QC criteria
• daily checks
• measure pH of a grab sample taken at the same
  location as in-line monitor, or
• check directly with a buffer
• compare measurements,
• difference should be no more
• than 0.2 pH

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Field Measurements - TRC

• Grab - Total Residual Chlorine
• EPA approved methods are
• DPD, colorimetric (most common)
• recommended for levels 0.2-4.0
• titration colorimetric
• titration amperometric - when DPD not applicable
• or feasible (e.g., color interference, low
  Cl level)
• color wheel comparators are not allowed for
• wastewater samples

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Field Measurements - TRC cont.

• Calibration and daily checks for DPD colorimetric
  method
• instrument spectrophotometer / photometer that
  can be calibrated with a blank and at least one
  standard
• confirm manufacturer calibration with a blank and
  three primary (chlorine or potassium
  permanganate) standards
• check meter daily with at least one gel standard
  and every six months with primary standards
• check gel standards quarterly against primary
  standards

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How to verify your meter
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Field Measurements - TRC cont.

• Total Residual Chlorine Analyzer
• initial calibration
• before installation and
• each time the instrument is taken off-line
• after fails QC criteria
• daily checks
• measure TRC of a grab sample taken at the same
  location as in-line analyzer, or check directly
  with a standard
• compare measurements, difference should be no
  more than 20 between meters (10 if check
  directly with a standard)

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Field Measurements - Turbidity

• Meter specifications per EPA Method 180.1
• Calibration requirements
• follow the manufacturers operating instructions
• primary (formazin) or secondary (gel type)
  standards can be used for daily checks or
  calibrations
• run at least one standard that fits within the
  field range needed
• secondary standards must be checked quarterly
  against a primary standard

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Field Measurements - Turbidity

• In-line Turbidimeter
• initial calibration
• before installation and
• each time the instrument is taken off-line
• after fails QC criteria
• daily checks
• measure turbidity of a grab sample taken at the
  same location as in-line analyzer or, measure a
  standard in the same range
• compare two measurements, difference should be no
  more than 20 (10 if checked with a standard)

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Field Measurements - Dissolved Oxygen

• Follow SOP FT 1500
• use a membrane/electrode DO meter with accuracy
  of ? 0.2 DO mg/L and sensor with automatic
  temperature compensation
• check calibration against the Oxygen Solubility,
  SM Table 4500-OI the difference should not
  exceed 0.3 mg/L
• before use check the meter in water-saturated air
• periodical checks against Winkler method may be
  required
• keep records of the calibrations, checks , sample
  measurements
• check in-line continuous DO meter daily (or as
  often as reported on the DMRs) against a second
  meter the difference should be no greater than
  0.2 mg/L

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Field Measurements - Specific Conductance

• Follow SOP FT 1200
• use meter with platinum or graphite electrode and
  temperature sensor
• calibrate the meter check with a standard,
  difference no more than 5
• keep records of calibrations, sample
  measurements, and temperature
• make sure to perform a temperature correction to
  25oC using formula given in the SOP (if not done
  automatically)
• check in-line continuous conductivity meter daily
  (or as often as reported on the DMR) against a
  second meter the difference should be no greater
  than 10

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Field Measurements - Temperature

• Follow the DEP SOP FT 1400
• field instrument must be capable of measuring
  temperature in 0.1oC increments
• types of thermometric devices digital
  thermistor, glass bulb mercury or alcohol filled,
  BI-metal strip, or advanced silicon chip
  temperature sensor
• check device against an NIST-traceable
  thermometer temperature should agree within
  ?0.1oC
• determine the maximum time between continuing
  verifications based on the instrument stability
  (EPA requires annual check)
• keep records of calibrations/checks and samples
  measurements
• additional EPA requirements
• thermistors should be checked against an NIST
  traceable thermometer prior to use and should
  agree within 4.0 C. This includes, but is not
  limited to the pH, conductivity, and DO meters.

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Records

• Records of calibration procedures
• date and time and location of the calibration and
  a field check if applicable
• name of the person performing calibration
• standards and pH buffers used
• actual reading of buffers / standards after the
  calibration
• corrective actions if applicable
• meter name and model number
• Reagent and standards documentation
• date and time of the receipt, expiration dates
• if any standard or chemical is used after the
  expiration date, there must be a documentation
  showing that the reagent is providing an
  acceptable response

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More Records

• Records of field measurements
• retain all original records
• date and time the measurement was collected
• location of the sample
• sample value and unit
• initial of the person taking the measurement
• Records of daily comparability checks
• date and time
• location
• reading from the continuous meter
• reading from the second meter
• difference no greater than 20 (turbidity and
  TRC)
• difference no greater than 0.2 pH units
• name of the person performing the check

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Summary Field Testing

• Field test methods
• Hand-held field meters
• In-line, continuous meters
• Calibration requirements
• Daily checks of in-line meters
• Records
• calibration procedures
• daily checks
• comparability checks
• sample measurements
• standards

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QA Plans for Field Procedures

• FA 1000 (FA 3300, Specific Section)
• Explanation
• Certification for Field Procedures-Future

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Up and ComingNew Draft QA Rule and SOPs

• Draft QA rule
• http//www.dep.state.fl.us/labs/qa/draftrulesop/in
  dex.htm
• Draft SOPs
• http//www.dep.state.fl.us/labs/qa/draftrulesop/so
  ps.htm

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Up and Coming Changes to DEP SOPs

• Field Residual Chlorine (FT 2000)
• Instruments with pre-set or factory
  calibration-verify with primary standards at
  least annually.
• Determining or verifying the values of
  secondary standards (gels)-at minimum annually.
• Unless standards have been damaged, stored in
  direct sunlight, failed to verify adequately, or
  if required to do more frequently by permit.
• Grab vs. Composite (FS 2000)-Definitions

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Any Questions And remember you can always call
us.