Title: Sampling and Field Testing at Wastewater Facilities Presented by Jenny Farrell and Debra Knight
1Sampling and Field Testing at Wastewater
FacilitiesPresented by Jenny Farrell and Debra
Knight
2Overview
- 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
3Where 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
4Which 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
5Sampling 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
6Sampling 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
7Sampling 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
8How 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
9Sampling Equipment
- Select sampling equipment
- buckets, spatulas, dippers, tubing, etc.
- Table FS 1000-1 and FS 1000-2
10Sampling 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.
11Tips 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.
12Tips 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
13Bacteria 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
-
-
14Sample 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
15Sample 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
16Residuals 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
17Sampling 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
18Field 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
19Field 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
20Measuring 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)
21Field 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
22Field 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
23Field 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
24How to verify your meter
25Field 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)
26Field 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
27Field 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)
28Field 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
29Field 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
30Field 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.
31(No Transcript)
32Records
- 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
33More 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
34Summary 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
35QA Plans for Field Procedures
- FA 1000 (FA 3300, Specific Section)
- Explanation
- Certification for Field Procedures-Future
36Up 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
37Up 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
38Any Questions And remember you can always call
us.