DEP Quality Assurance Requirements for Sample Collection &

DEP Quality
Assurance
Requirements for
Sample Collection &
Field Testing
Department of Environmental Protection
Environmental Assessment Section
Bureau of Laboratories
Why Use the SOPs?
† QA Rule – Chapter 62-160, F.A.C.
† DEP SOPs for Field Activities
„ Sample Collection
„ Preservation & Holding Times
„ Mandatory Documentation
„ Quality Control
„ Field Measurements
† CERP QASR
Where to Find:
www.dep.state.fl.us/labs/sop/index
Department of Environmental Protection
Standard Operating Procedures for Field
Activities
DEP-SOP-001/01
Use for:
Training and Daily Use
FLORIDA DEPARTMENT OF ENVIRONMENTAL PROTECTION
2600 BLAIR STONE ROAD
TALLAHASSEE, FL 32399-2400
Bureau of Laboratories
Environmental Assessment Section
February 1, 2004
1000
General Sampling
FS
Field Sampling
2000
General Aqueous
General
Direct Grab
2000
Aqueous
2100
Surface Water
Surface Grabs
Intermediate Devices
3000
Soil
2200
Groundwater
Water Depth Grab
Pumps
4000
Sediment
2300
Drinking Water
Automatic Samplers
5000
Waste
2400
Wastewater
6000
Biological Tissue
7000
Biological
DEP SOP Structure
Naming Conventions
8000
Miscellaneous
FA
FC
FS
FM
Administrative & Quality Systems
Field Cleaning
Sampling Procedures
Mobilization & Laboratory
FQ Quality Control
FD Documentation
FT Field Testing
Key Sampling
Considerations
Data Quality Objectives
Representative Samples
Sample Integrity
Documentation
Administrative Approvals &
Quality System Management
† Intent and purpose of the SOPs
† Description of SOP format
† Regulatory requirements for use of the SOPs
† Approval of alternative field procedures
† Quality system management guidelines
† Proficiency requirements for biological
sampling
† Field performance audit checklists
† Definitions for matrices, analytes, other
terms
FD 1000
Quality System
† Must Have a Quality Manual
„ Quality System Design
„ QA Policy and Procedure
„ QA Personnel Functions
† Available upon Request
FA 3000
Auditing
†
You may be audited by External
Organizations!!
„
„
†
Sampling Performance (Field Audit)
Data Usability (Documentation Audit)
Audit Criteria
„
„
„
DEP SOPs
Any approved alternative procedures
Project Data Quality Objectives
Internal Audits Recommended
† Guidance checklists in Appendix to FA 1000 or at:
† http://www.dep.state.fl.us/labs/library/index.htm
†
FA 4000
Documentation
† Universal record-keeping requirements
† Required records for each DEP SOP
† Requirements also apply to:
„ Electronic (digital) data
„ Video, film, maps, other media
† Documenting transmittal to labs or others
† Evidentiary (legal) chain-of-custody
† Example forms
FD 1000
Good Documentation Habits
for Verification and
Defensibility
† Records must be:
„ Intact & easily understood
„ Linked to all field data and
analytical result
† Note & correct errors without obliteration
† Signature or initials indicate functions and
responsibilities
† Retain records for 5 years after project
completion (Legal Cases Longer??)
“When in doubt, write it down”
FD 1000
Typical Facts to Record
†
†
†
†
†
†
†
†
†
†
†
†
†
†
†
†
†
Unique identification of sample containers (analyte group)
Number of sample containers for each unique container identification
Site and sampling point identification and matrix
Sample type (grab, composite, equipment blank, trip blank, etc.)
Sampler names, initials or signatures
Sample collection date, time, depth, flow rate
Sample preservation and preservation checks
Notes about sample problems
Ambient field conditions
Monitor well purging and stabilization log
Sampling and purging equipment used
Equipment decontamination log
Equipment maintenance log
Field testing measurements
Field meter calibration records
Links with site maps, videos, photos
Transmittal of samples to lab or other party
FD 1000
Decontamination
†
†
†
†
†
†
†
“Performance-Based” Cleaning
Cleaning Reagents & Analyte-Free Water
General Cleaning Procedures
Cleaning Specific Equipment Types
Sample Container Cleaning
Cleaning Heavily Contaminated Equipment
Cleaning Procedure Tables in Appendix
FC 1000
Performance-Based Cleaning
† Cleaning must:
„ Be Effective
„ Use non-contaminating techniques
† Demonstrate Effectiveness with
Blanks and other QC
† Suggested Procedures in
Appendix
Cleaning to
meet a set of
specifications
rather than
following a
rigid, required
procedure
FC 1000
Mandatory Sampling QC
† Handle and Document Exactly
like the Associated
Environmental Samples:
† Sampling QC Blanks
Required for:
„
„
„
„
„
„
„
„
Volatile Organics
Extractable Organics
Metals and Ultra-Trace Metals
Inorganic Non-Metallics
Radionuclides
TRPH, FL-PRO and Oil & Grease
Volatile Inorganics
Aggregate Organics (except
BOD, cBOD)
„
„
„
Unique Container ID
Preservation
Documentation
‡
‡
‡
‡
‡
‡
„
„
Type of QC sample
Date and time of collection
Preservatives used and preservation
checks
Type & source of analyte-free water
for blanks
Sampling equipment used to collect
QC sample
Procedure used to collect QC sample
Transport
Storage
† Link QC sample records with the
associated environmental
sample documentation
FQ 1200
Mandatory Blank
Frequencies
† 5% equipment blanks per matrix and
analyte for each project
† 5% field blanks per matrix and analyte
each project (if no equipment used)
† One equipment blank or field blank per
matrix and analyte per year for each
project
† Trip blank in each ice chest (each trip)
FQ 1230
Equipment Blanks
† Collect
Pre-Cleaned
Equipment Blank before
Equipment is used during
the Sampling Event
† Collect Field-Cleaned
Equipment Blank after
Equipment is Cleaned
during the Sampling
Event
†Collect on-site: rinse sampling equipment (including
filtration equipment) with analyte-free water
FQ 1200
Field Blanks
† Use when an environ-
mental sample is
collected with the
sample container
(no other equipment
used for collection
of the sample)
† Collect on-site: pour analyte-free water into
clean sample containers
FQ 1214
Trip Blanks (VOCs Only)
Lab or field team fills VOC vials
with analyte-free water before
sampling trip
† Handle same as VOC samples
†
„
„
Accompanies empty VOC vials & VOC
samples (shipment, transport &
storage)
One trip blank in each ice chest or
shipping (transport) container
Prepare trip blanks for each
sampling trip
† Remain sealed (unopened) until
analysis
†
FQ 1213
General Sampling Procedures
†
†
†
†
†
†
†
†
†
†
General Cautions and Instructions
Cross-Contamination Prevention
General Procedure for Composite Samples
Sample Container and Equipment Rinsing
Placement of Fuel-Powered Equipment
Sample Preservation and Preservation Checks
Preventive Maintenance of Equipment and Instruments
Handling Hazardous and Site-Derived Waste
Sample Custody and Tracking Procedures
Tables:
„
„
Sample Preservation, Holding Times & Container Types
Construction Materials & Approved Sampling Equipment
FS 1000
Table FS 1000-2
† Acceptable Materials to be
Used for Each Analyte
Group
Equipment Type and Construction
† Permissible Analyte Groups for
Each Equipment Type
† Restrictions & Precautions for Using
Specific Equipment Configurations
†
Table FS 1000-3
CONSTRUCTION
TUBING
HOUSING
EQUIPMENT
Surface Water
Intermediate containers such as
SS, Teflon, Teflon- N/A
pond sampler, scoops, beakers, coated, HDPE,
buckets, and dippers
PP
Glass
N/A
Non-inert
Nansen, Kemmerer, Van Dorn,
Alpha and Beta Samplers,
Niskin (or equivalent)
N/A
SS, Teflon, Teflon- N/A
coated, HDPE,
PP
Non-inert
N/A
USE
Grab sampling
PERMISSIBLE ANALYTE GROUPS
RESTRICTIONS AND PRECAUTIONS
All analyte groups
None
All analyte groups except boron and
fluoride
All analyte groups except volatile and
extractable organics
Specific depth grab All analyte groups
sampling
None
None
None
All analyte groups except volatile and
extractable organics
All analyte groups
None
None
DO Dunker
SS, Teflon, glass, N/A
HDPE, PP
Water column
composite sampling
Bailers – double valve
SS, Teflon, HDPE, N/A
PP
Non-inert
N/A
Grab sampling
All analyte groups
None
Grab sampling
All analyte groups except volatile and
extractable organics
SS, Teflon, Specific depth
PE, PP
sampling
All analyte groups except volatile and
extractable organics
None
If sampling for metals, the tubing must be
non-metallic if not SS
Silicone tubing in pump head
Must be variable speed
Peristaltic pump
N/A
Extractable organics
N/A
Non-inert
All analyte groups except volatile and
extractable organics
; configured as specified in Figure FS
1000-1, or use tubing constructed with
approved materials in the pump head
Silicone tubing in pump head
Must be variable speed
Tables FS 1000-1 to 1000-3
† Equipment Type and
Construction
† Permissible Analyte
Groups for Each
Equipment Type
† Restrictions &
Precautions for Using
Specific Equipment
Configurations
Tables FS 1000-4 to 9
†
†
†
†
†
†
Preservation,
1000-4:
40 CFR PartHolding Times, Containers
136 Table II
1000-5: Analytes Not
Listed in 40 CFR Part
136
1000-6: Sediments,
Soils & Residuals
1000-7: Soil VOCs
(SW 846, Method
5035)
1000-8: Exceptions
for Drinking Water
1000-9: Biosolids
Contamination
Prevention
†
†
†
†
†
†
†
Rinse all sampling equipment with sample water
before collecting samples and discard rinse
water away from sampling point
Do not rinse sample containers for O&G, TRPH, FL-PRO, microbiology
or containers pre-dosed with preservatives
Collect from least to most contaminated source
Collect upwind and away from fuel-powered equipment
Keep equipment, containers and supplies clean until use
Don’t put pump tubing, meter probes, other implements or fingers into
sample containers
Segregate:
„
„
Highly contaminated samples
Incompatible samples
Keep ice chests and other transport containers clean between
sampling trips
† Change gloves between sampling points or sources and if torn or
contaminated
†
FS 1002
General Aqueous
Sampling
General Collection, Filtration and Preservation
Procedures for Aqueous Samples
† Instructions for Specific Analyte Groups
†
„
„
„
„
„
„
„
Metals
Extractable Organics (SVOCs)
Volatile Organics (VOCs)
Bacteria Samples
Hydrocarbons (O&G, TRPH, FL-PRO)
Radioisotope Samples and Radon
Cyanide Samples
FS 2000
Preserving Samples
† Dechlorinate and/or filter (if applicable) before
†
†
†
†
†
†
†
†
†
preserving
Preserve per tables FS 1000-4 through FS 10009
Preserve immediately (within 15 minutes of
collection)
Use ice to keep samples @ 4ºC
Check pH of pH-preserved samples (see check
frequencies in FS 2000) with narrow range pH
paper (including pre-preserved containers)
Don’t dip pH paper into the sample
pH checks not required for VOCs
Carry and add extra preservative if required by
pH check
Avoid excess preservative (can dilute sample or
cause analytical problems)
Use refrigeration or ice for automatic samplers
FS 2000 & FS 2001
Filtering
Samples
† Perform on-site
† Pore size & filter type:
„ 0.45 ȝm
† Filtration may be a
preservation requirement
† Filter groundwater samples for metals only
after DEP site-specific approval
† Filter before chemical preservation or
chilling
FS 2000
Collecting VOC
Samples
†
†
†
†
†
†
†
†
†
†
Teflon-coated silicone cap liner
(septum)
Prevent contamination from fuel sources
Do not open VOC vial until ready to fill
No aeration or agitation of sample
Reduce flow from pumps or faucets to ”100 mL/min
Dechlorinate per SOP instructions and restrictions
Do not overfill pre-preserved vials
Do not pour sample into vial cap
No headspace in VOC vial after collection
Do not re-open vials to refill or to remove bubbles
(” 5mm total bubble diameter OK)
FS 2004
Sampling for Bacteria
† Collect last (short holding time)
† Sterilized containers required
† Use dechlorinating agent (if
†
†
†
†
†
applicable)
Thoroughly rinse any
intermediate devices
Keep fingers away from
container opening
Don’t underfill or overfill
whirlpaks
Close whirlpaks securely
Cool immediately with wet ice
FS 2005
Sampling for
Hydrocarbons
(Oil &Grease, TRPH, FL-PRO)
† Do not skim surface of water (unless required
by sampling plan)
† Do not pre-rinse bottles with sample
† Do not use automatic samplers
† Preserve with sulfuric or hydrochloric acid
and chill
FS 2006
FS 2100 Surface Water
FS 2400 Wastewater
† Common Procedures
† General Cautions
† Equipment Selection
† Grab and Composite Definitions
† Sampling Techniques
Surface & Depth Grab Samples
„ Manual or Automatic Composite Samples
„
Sampling Strategies
†
Collect
„
„
„
„
„
†
Least to most contaminated
‡ Downstream to upstream
‡ Bow of the boat
Upwind and away from fuel sources
Upstream and away from body
Don’t suspend bottom material into water column
Sample water before collecting sediments
Consider:
„
„
„
„
Location relative to artificial structures
Permit-specific sampling points
Flow characteristics of sample source
Heterogeneity or homogeneity of sample source
FS 2100 & FS 2400
Representative
Sampling and
Contamination Prevention
†
†
†
†
†
†
Mix discrete sub-samples thoroughly prior to manual
compositing
Avoid cross-contamination between sampling points
Clean reusable equipment appropriately
Collect field QC blanks as applicable
Flush wastewater taps to remove settled solids and
reduce flow before sampling
Dechlorinate wastewater samples when required
„
VOCs, extractable organics, microbiology, cyanide
FS 2100 & FS 2400
Grab Samples
Use As:
Discrete sample
collected over a
period of time not
exceeding 15
minutes
† Snapshot in time
† Direct observation of
†
†
†
†
†
†
†
conditions at time of
sampling
Intermittent flows
Constant waste stream or
water body characteristics
Batch discharges
Determining min/max
concentrations
Tracing slug loads or spills
Analytes with short holding
times
Analytes altered by
composite techniques
FS 2110, FS 2420 & FS 2430
Using a Sample Container
† Do not use pre-preserved containers
„ Use intermediate sampling device in this case
† Sample is collected directly into sample
container by hand
„
Pole extensions may be used
† Collect surface samples within top 12” of
water column
„
„
„
Sampling plan may require greater depth
Avoid skimming unless required by sampling plan
Direct container grab preferred over intermediate
devices
FS 2110 & FS 2430
Using Intermediate Devices
† Restrictions:
„
„
Avoid O&G, TRPH, FL-PRO
Appropriate construction materials
‡ Rinse with site water
–
Discard rinses away
from & downstream
of sample location
FS 2100 & FS 2430
Grab Samples at Depth
† Equipment selection is dependent on project
objectives and analyte groups
† Water column depth is measured and
recorded
† Sampling point depth is
accurately determined
and recorded
† Bottom sediments are not
disturbed
FS 2110 & FS 2430
Using Pumps
†
†
†
†
†
†
Proper configuration and
construction materials
Do not collect O&G, TRPH &
FL-PRO
Do not pull organics through
peristaltic pump head
Flush pump and tubing with
3 volumes of sample water
Anchor intake at calculated
depth
Record depth of intake
FS 2110, & FS 2430
Composite Sample:
A sample collected over time,
taken either by continuous
sampling or by mixing discrete
samples. Composite samples
reflect the average
characteristics during the
compositing period
†
†
†
†
†
†
†
Use if:
Continuous flow
Limited analytical capacity
Average analyte concentration
over time
Calculating mass/unit time
loadings
Correlation of concentration
data with flow
Reduction of sampling errors
and hazard exposure with use
of autosamplers
Unattended sampling with
autosamplers
FS 2110, FS 2410, FS 2423 & FS 2430
Groundwater
General Considerations:
† Fresh Formation (aquifer)
Water Must be Collected
† Amount of Water Purged Determined by
Well Conditions
„
Parameter-driven Completion Criteria
† Bailers Not Recommended
„ Specific Techniques Must be used
FS 2200
General Purging
Procedures
†
†
†
†
†
†
Avoid dropping anything to the bottom of well
Ensure proper pump or
tubing placement in well
and record placement depth
Measure water level frequently
during purging and stabilize
drawdown with pump rate
Purge required minimum
volumes
Measure parameters at proper frequency
Satisfy purge completion criteria
FS 2213
Purging with a Pump
† Place Intake at Correct Depth
† Stabilize Drawdown with Pump Rate
† Purge Required Minimum Volumes
† Measure Parameters at Proper
Frequency
† Satisfy Purge Completion Criteria
Conventional Purge
To Pump
†Intake placed at the top of
water column
„
„
„
Water
Level
Purge at least 1½ well volumes
Intake
Screened
Interval
Calculate well volume
Purge one well volume
Measure stabilization
parameters no sooner than
each ¼ well volume interval
Minimized Purge Volumes
To Pump
†Well screen length ”10 feet
†Configuration used for both
purging and sampling
†Intake or pump placed at midscreen
†Calculate equipment volume
†Purge one equipment volume
†Measure stabilization parameters
†Collect additional measurements
no sooner than every 2 minutes
Water
Level
Purge a minimum of 3
equipment volumes
Screened
” 10 ft
Interval
Intake
FS 2212 & FS 2213
Partially Submerged Screen
To Pump
† Intake placed at ½ distance
†
†
†
†
between top of water column
and bottom of screen
Calculate well volume
Purge one well volume
Measure stabilization
parameters
Collect additional
measurements no sooner than
every 2 minutes
Water
Level
Screened
Interval
Intake
Purge a minimum of
1 Well Volume
FS 2212 & FS 2213
Use a Flow-Through Cell
Purging
Completion Criteria
† Three consecutive Measurements
„
„
„
„
„
Temperature: ± 0.2° C
pH: ± 0.2 Standard Units
Specific Conductance: ± 5.0% difference
Dissolved Oxygen: ” 20% Saturation
Turbidity: ” 20 NTU
or
† Three Consecutive Measurements:
„
„
„
„
„
Temperature: ± 0.2° C
pH: ± 0.2 Standard Units
Specific Conductance: ± 5.0% difference
Dissolved Oxygen: ± 0.2 mg/L or ±10%,
whichever is greater
Turbidity: ± 5 NTU or ±10%, whichever is greater
FS 2212
Maximum (Default) Purge
Volumes
† Five Well Volumes only if
Stabilization Measurements Fail
„ Proper Techniques Verified
„ Project Manager Approval
„
† One Fully Dry Purge (only for low
recharge at < 100 mL/min pump rate)
Purging and Sampling
Low-Recharge Wells
†
†
†
†
†
†
†
†
†
†
Minimize equipment volume
Use thick-walled tubing
Use same equipment for purging and sampling
Place intake at mid-screen depth
Purge < 100 mL/min
Purge 2 equipment volumes
Measure parameters just before sampling
Keep pump at the purge position
Keep pumping rate the same (unless purged dry)
Collect samples immediately after purging (or after
dry recharge if purged at < 100 mL/min)
FS 2212 & FS 2222
Maximum Time Between
Purging & Sampling
† Re-measure parameters > 1 hour after
purging
† Re-purge if parameters > 10% of original
† Dry-purge wells sampled immediately after
sufficient recharge & parameter
measurement
† All samples collected within 6 hours of
purging
FS 2212
Purging & Sampling
Wells with Installed
Plumbing
† Purge System until Stable (pH, DO,
Turbidity, Temperature and Specific
Conductance)
† Reduce flow to ” 500 ml/min (” 100
mL/min for VOCs)
† Collect samples directly into sample
containers
FS 2214, FS 2215 & FS 2223
Sediment Sampling
† Base equipment selection on sample
type and analytes of interest
† Sampling locations should allow a
representative portion of the sediment
to be collected with minimal
disturbance
† Collect surface water samples before
beginning sediment sampling
FS 4000
Scoops
† Most useful around the
margin or shore of the
water body or by wading in shallow waters.
† Take precautions not to disturb the bottom
prior to scooping.
† Scoop the sample in the upstream direction
of flow.
† There are ways to modify scoops.
FS 4000
Cores
†
†
†
†
†
Use only appropriate construction materials for
corers and liners.
Cores preserve historical sediment layering.
Water displacement is minimal (minimizes the shock
wave produced by other equipment such as
dredges).
Good for sampling fine sediments in static waters,
especially those containing trace organics and
metals.
Sample washout can be a problem: prevent!
„
„
Nosepiece or core-catcher at bottom
Check-valve at top
FS 4000
Dredges
†
Make sure the jaws fully close!
„
„
Ponar - hard or rocky substrates, in
deep water bodies, or streams with
fast currents
Eckman - soft, mucky sediments
Ponar
Eckman
Peterson
FS 4000
Soil Sampling
Select sampling equipment based on the type of
sample to be collected and the analytes of interest.
† Choose locations such that a representative portion
of the soil is collected with minimal disturbance.
† Locations where stressed or dead natural vegetation
and/or areas with surficial soil staining may indicate
improper waste disposal practices.
† Attempt to match background sample soil types
(e.g., sands vs. clays) with the site soil
characteristics.
†
FS 3000
Composite Sampling
†
Composite soil samples in the laboratory, not the
field.
„
„
Soil composites depend on the project DQOs
Design composite scheme per project objectives
Select sampling points for each aliquot or subsample
† Record the amount of each aliquot
† Recommended:
†
„
„
Do not mix sample aliquots before containerizing
Request mixing of unmixed composite sub-samples by lab
FS 3000
Surface Soil Sampling
†
Surface soil
„
Soil between the ground
surface and 6-12 inches
below ground surface
Remove leaves, grass
and surface debris from
the area to be sampled.
† Select an appropriate precleaned sampling device
to collect the sample.
†
FS 3000
Subsurface Sampling
† Interval begins at
approximately 12 inches
below ground surface.
† DEP Recommended
(resulting in minimal
disturbance to the sample):
„
„
Core Barrel
Split Spoon Sampler
† Other methods:
„
„
„
„
„
Shovels and Diggers
Backhoe
Bucket Augers and Hollow
Corers
Direct Push
Shelby Tube Sampler
FS 3000
FT 1000 – FT 3000
Field Testing
† pH
† Specific
Conductance
† Temperature
† Dissolved Oxygen
† Turbidity
† Residual Chlorine
†
†
†
†
†
†
†
†
†
†
Water Flow
Sediment Oxygen
Demand
Dissolved Gases
Salinity
Transparency
Continuous
Monitoring
Sulfite
Aquatic Habitat
Characterization
ORP
Combustible Gases
General Field Testing
Requirements
† Measurement Concepts
„ Initial calibration of instruments
„ Verification per acceptance criteria
„ “Bracketing” sample tests with verifications
† General Requirements for Calibrations
† General Requirements for Verifications
† Documentation Requirements
„ Calibrations
„ Verifications
„ Sample Measurements
FT 1000
Field Testing Concepts
† Calibration: Manually or Automatically
Adjusting Electronics
Measure Calibration
Calibrate
(Adjust) Instrument
Standard
Display Value
with Instrument
Calibrations can only occur at the beginning of a
chronological bracket
FT 1000
Field Testing Concepts
Verification: Checking the Instrument with Known
Standard Value to Verify Instrument Response
Not Acceptable
† Measure a Standard as if it was a Sample
† Compare Result with Acceptance Criterion
† Accept or Reject Verification
Acceptable
Meter Readings
FT 1000
Field Testing - Bracketing
Chronological Bracket
Initial calibration = 10:00 AM
Sample measurement = 10:15 AM
Calibration verification = 10:30 AM
Quantitative Range Bracket
Standard A: pH = 7.0
Standard B: pH = 10
pH in Sample: = 7.5
Standard A: 100 umhos/cm
Standard B: 1000 umhos/cm
Sample = 400 umhos/cm
FT 1000
Out of Quantitative
Bracket Range
Standard A: pH = 7.0
Standard B: pH = 10
pH in Sample: = 6.5
Standard A: .18 mg/L Cl
Standard B: 1.5 mg/L Cl
Sample = 3 mg/L Cl
Report any Sample Values that are Outside the
Range of the Standards as Estimated (“J”)
or
Verify Calibration with Additional Standard to
Include Sample in Quantitative Bracket:
Standard C: pH = 4.0
Standard C = 4 mg/L Cl
FT 1000
Calibration/Verification/Measurement
Sequence
“Calibrate” Mode
Begin with a Standard
Calibrate or adjust instrument
Calibrate or adjust instrument
Choose 2nd Standard
“Read” (Verification) Mode
Measure
Verification Standard
Verification acceptable?
YES
Verify with
different
Standard
Out of
Standard
Range?
Measure samples
NO
Repeat
Verification
Or Perform
Cal.
Calibration Verification
Frequency
† Perform Verification Before Measuring
Samples
† Perform Verification at End of Use or at 24hour Intervals (initially)
† Extended Verification Intervals up to One
Month are Acceptable if Instrument Stability
is Documented
† Temperature Verifications Can Be Further
Extended
FT 1000
Secondary Standards
† For Chlorine and Turbidity
† Typically Manufacturer
-specific
† Field-rugged for Routine use
„
„
„
Store Upright
Protect from Sun
Protect from Extreme
Temperatures
† Discard when no longer
verifiable
FT 1000
Verifying Secondary
Standards
† Use Same Instrument
† Use only Standards that meet Manufacturer’s and SOP
requirements
† Verify at least Quarterly
† Verify Using Primary Standard(s)
„
Include a Blank for TRC
† “READ” Each Secondary Standard
† You may need to assign values the first time you verify
secondary standards. - Read and follow the mfg
instructions
† Instrument Value must be within
„
„
SOP-Specified Range of the Stated or Assigned Value and
The Manufacturer’s Tolerance Range
Only Use Secondary Standards for Verification
FT 1600 & 2000
Continuous Monitoring Devices
In-Line Instrument
† Calibrate:
„ Before First Installation
„ When Verifications are not acceptable
† Verify
„ After Every Calibration
„ After Preventive Maintenance Activities or
„ When Taken Off line
† Use Primary Standards
FT 1900
Continuous Monitoring Devices
Indirect Verification
†
Verifications
„
„
Perform at least monthly or
At Intervals to ensure Continuing Acceptance
Collect Sample at Same Point that Instrument Sensor
is Deployed
† Analyze Sample using Selected Test Method
† Compare Results with Monitor Reading
† Value must be within SOP Verification Requirements
†
FT 1900
Checking Your Technique
Dissolved Oxygen (FT 1500)
Vent to atmosphere
Inspect membrane
Enclose with saturated air
Ensure stable temperature
Checking Your Technique
Dissolved Oxygen Verification (FT 1500)
Record Temperature
Record DO in mg/L
Table FS 2200-2
Dissolved Oxygen Saturation
TEMP
D.O.
deg C
SAT.
15.0
15.1
15.2
15.3
15.4
15.5
15.6
15.7
15.8
15.9
16.0
16.1
16.2
16.3
16.4
16.5
16.6
16.7
16.8
16.9
17.0
17.1
17.2
mg/L TEMP
20%
deg C
D.O.
SAT.
mg/L TEMP
20%
deg C
D.O.
SAT.
mg/L TEMP
20%
deg C
D.O.
mg/L
SAT.
20%
10.084 2.017 19.0
9.276
1.855 23.0
8.578
1.716 27.0
7.968
1.594
10.062 2.012 19.1
9.258
1.852 23.1
8.562
1.712 27.1
7.954
1.591
10.040 2.008 19.2
9.239
1.848 23.2
8.546
1.709 27.2
7.940
1.588
10.019 2.004 19.3
9.220
1.844 23.3
8.530
1.706 27.3
7.926
1.585
9.997 1.999 19.4
9.202
1.840 23.4
8.514
1.703 27.4
7.912
1.582
9.976 1.995 19.5
9.184
1.837 23.5
8.498
1.700 27.5
7.898
1.580
9.955 1.991 19.6
9.165
1.833 23.6
8.482
1.696 27.6
7.884
1.577
Table
1:
Solubility
of
Oxygen
in
Water
9.934 1.987 19.7
9.147
1.829 23.7
8.466
1.693 27.7
7.870
1.574
9.912 1.982 19.8
9.129 1,2 1.826 23.8
8.450
1.690 27.8
7.856
1.571
at Atmospheric Pressure
9.891 1.978 19.9
9.111
1.822 23.9
8.434
1.687 27.9
7.842
1.568
9.870 1.974 20.0
9.092
1.818 24.0
8.418
1.684 28.0
7.828
1.566
9.849
1.970
20.1
9.074
1.815
24.1
8.403
1.681
28.1
7.814
Temperature Oxygen Solubility Temperature Oxygen Solubility 1.563
9.829 1.966 20.2
9.056
1.811 24.2
8.387
1.677 28.2
7.800
1.560
o
o
C 20.3 9.039mg/L
C 1.674 28.3mg/L
9.808 1.962
1.808 24.3
8.371
7.786
1.557
9.787 1.957
20.4
9.021
1.804
24.4
8.356
1.671
28.4
7.773
1.555
0.0
14.621
26.0
8.113
9.767 1.953 20.5
9.003
1.801 24.5
8.340
1.668 28.5
7.759
1.552
1.0 20.6 8.985
14.216
27.0 1.665 28.67.968
9.746 1.949
1.797 24.6
8.325
7.745
1.549
9.726 1.945
1.794 24.7
8.309
7.732
1.546
2.0 20.7 8.968
13.829
28.0 1.662 28.77.827
9.705 1.941 20.8
8.950
1.790 24.8
8.294
7.718
1.544
3.0
13.460
29.0 1.659 28.87.691
9.685 1.937 20.9
8.932
1.786 24.9
8.279
1.656 28.9
7.705
1.541
4.0 21.0 8.915
13.107
30.0 1.653 29.07.559
9.665 1.933
1.783 25.0
8.263
7.691
1.538
9.645 1.929
1.780 25.1
8.248
7.678
1.536
5.0 21.1 8.898
12.770
31.0 1.650 29.17.430
9.625 1.925 21.2
8.880
1.776 25.2
8.233
1.647 29.2
7.664
1.533
Compare with Chart (Table FT 1500-1 or FS 2200-2)
60
12 447
32 0
7 305
Table FS 2200-2
Dissolved Oxygen Saturation
Temperature: 21.6
Reading: 9.08
Theoretical: 8.812
Difference: 0.268
TEMP
D.O.
D.O.
mg/L
deg C
SAT.
mg/L TEMP
20%
deg C
SAT.
D.O.
mg/L TEMP
20%
deg C
SAT.
D.O.
mg/L TEMP
20%
deg C
SAT.
20%
15.0
15.1
15.2
15.3
15.4
15.5
15.6
15.7
15.8
15.9
16.0
16.1
16.2
16.3
16.4
16.5
16.6
16.7
16.8
16.9
17.0
17.1
17.2
17.3
17.4
17.5
17.6
17.7
17.8
17.9
18.0
18.1
18.2
18.3
18.4
18.5
18.6
18.7
18.8
18.9
10.084
10.062
10.040
10.019
9.997
9.976
9.955
9.934
9.912
9.891
9.870
9.849
9.829
9.808
9.787
9.767
9.746
9.726
9.705
9.685
9.665
9.645
9.625
9.605
9.585
9.565
9.545
9.526
9.506
9.486
9.467
9.448
9.428
9.409
9.390
9.371
9.352
9.333
9.314
9.295
2.017
2.012
2.008
2.004
1.999
1.995
1.991
1.987
1.982
1.978
1.974
1.970
1.966
1.962
1.957
1.953
1.949
1.945
1.941
1.937
1.933
1.929
1.925
1.921
1.917
1.913
1.909
1.905
1.901
1.897
1.893
1.890
1.886
1.882
1.878
1.874
1.870
1.867
1.863
1.859
19.0
19.1
19.2
19.3
19.4
19.5
19.6
19.7
19.8
19.9
20.0
20.1
20.2
20.3
20.4
20.5
20.6
20.7
20.8
20.9
21.0
21.1
21.2
21.3
21.4
21.5
21.6
21.7
21.8
21.9
22.0
22.1
22.2
22.3
22.4
22.5
22.6
22.7
22.8
22.9
9.276
9.258
9.239
9.220
9.202
9.184
9.165
9.147
9.129
9.111
9.092
9.074
9.056
9.039
9.021
9.003
8.985
8.968
8.950
8.932
8.915
8.898
8.880
8.863
8.846
8.829
8.812
8.794
8.777
8.761
8.744
8.727
8.710
8.693
8.677
8.660
8.644
8.627
8.611
8.595
1.855
1.852
1.848
1.844
1.840
1.837
1.833
1.829
1.826
1.822
1.818
1.815
1.811
1.808
1.804
1.801
1.797
1.794
1.790
1.786
1.783
1.780
1.776
1.773
1.769
1.766
1.762
1.759
1.755
1.752
1.749
1.745
1.742
1.739
1.735
1.732
1.729
1.725
1.722
1.719
23.0
23.1
23.2
23.3
23.4
23.5
23.6
23.7
23.8
23.9
24.0
24.1
24.2
24.3
24.4
24.5
24.6
24.7
24.8
24.9
25.0
25.1
25.2
25.3
25.4
25.5
25.6
25.7
25.8
25.9
26.0
26.1
26.2
26.3
26.4
26.5
26.6
26.7
26.8
26.9
8.578
8.562
8.546
8.530
8.514
8.498
8.482
8.466
8.450
8.434
8.418
8.403
8.387
8.371
8.356
8.340
8.325
8.309
8.294
8.279
8.263
8.248
8.233
8.218
8.203
8.188
8.173
8.158
8.143
8.128
8.114
8.099
8.084
8.070
8.055
8.040
8.026
8.012
7.997
7.983
1.716
1.712
1.709
1.706
1.703
1.700
1.696
1.693
1.690
1.687
1.684
1.681
1.677
1.674
1.671
1.668
1.665
1.662
1.659
1.656
1.653
1.650
1.647
1.644
1.641
1.638
1.635
1.632
1.629
1.626
1.623
1.620
1.617
1.614
1.611
1.608
1.605
1.602
1.599
1.597
27.0
27.1
27.2
27.3
27.4
27.5
27.6
27.7
27.8
27.9
28.0
28.1
28.2
28.3
28.4
28.5
28.6
28.7
28.8
28.9
29.0
29.1
29.2
29.3
29.4
29.5
29.6
29.7
29.8
29.9
30.0
30.1
30.2
30.3
30.4
30.5
30.6
30.7
30.8
30.9
7.968
7.954
7.940
7.926
7.912
7.898
7.884
7.870
7.856
7.842
7.828
7.814
7.800
7.786
7.773
7.759
7.745
7.732
7.718
7.705
7.691
7.678
7.664
7.651
7.638
7.625
7.611
7.598
7.585
7.572
7.559
7.546
7.533
7.520
7.507
7.494
7.481
7.468
7.456
7.443
1.594
1.591
1.588
1.585
1.582
1.580
1.577
1.574
1.571
1.568
1.566
1.563
1.560
1.557
1.555
1.552
1.549
1.546
1.544
1.541
1.538
1.536
1.533
1.530
1.528
1.525
1.522
1.520
1.517
1.514
1.512
1.509
1.507
1.504
1.501
1.499
1.496
1.494
1.491
1.489
Derived using the formula in Standard Methods for the Examination of Water and Wastewater, Page 4-101, 18th Edition, 1992
Checking your Technique
pH (FT 1100)
† When Calibrating, always begin with
a pH 7 buffer
† Rinse Probe with DI
Water between
Measurements
Check your Technique
Turbidity (FT 1600)
† Only Calibrate a Turbidity-free Water
Blank and Primary Standards
„
Formazin or Styrene divinylbenzene
† Verify Calibration with Primary
Standard
† Verify Secondary Gel Standards
Quarterly
„
Verify with a Primary Standard before
“reading” the Gel Standards
Check your Technique
Specific Conductance (FT 1100)
† Select Standards that bracket the
range of sample measurements
† A 100 umho/cm standard is acceptable
verification for any sample below 100
umho/cm
Calibration Records
Standards
† Manufacturer’s Name
† Lot Number
† Expiration Date
† Concentration
„
Range (if applicable)
FT 1000
Calibration Records
Dissolved Oxygen
† Verification reading (mg/L)
† Verification temperature (C)
† Expected saturation value (mg/L)
† Calculated Deviation from Expected
Saturation Value
FT 1000
Calibration Records
pH and Specific Conductance
† pH
„
„
„
„
Calibration buffer values
Verification buffer expected value
Meter reading of verification buffer
Calculated deviation from expected value
† Specific Conductance
„
„
„
„
Calibration standard value
Verification standard expected value
Meter reading of verification standard
Calculated % deviation from expected value
FT 1000
Calibration Records
Turbidity & Residual Chlorine
† Primary Calibration Standards
Standard Values
„ Expected Value(s) of Primary Standard
used for Verification
„ Instrument Reading of Verification
Standard(s)
„ Calculated % Deviation of Readings from
Expected Value(s)
„
FT 1000
Calibration Records
Turbidity & Residual Chlorine
† Records when Assigning Values or Verifying
Secondary Standards
„
„
„
„
„
Previously Assigned 2ndary Standard Value or
Manufacturer’s Stated Value
Current Reading from Instrument
Calculated Deviation between Current Reading
and Previous Value
New Value assigned from Current Reading (if
applicable)
Manufacturer’s Tolerance Range (for Residual
Chlorine)
FT 1000
Calibration Records
Turbidity & Residual Chlorine
† Records when Verifying with
Secondary Standards
Verification Standard Value(s) (expected
values)
„ Reading from 2ndary Standard(s)
„ Calculated % Deviations from Expected
Verification Values
„
FT 1000
Field Testing Acceptance Criteria per DEP-SOP-001/01
Parameter
Acceptance Criteria
pH
+ 0.2 Standard pH Units of calibration buffer
Specific Conductance
+ 5% of calibration standard value
Dissolved Oxygen
+ 0.3 mg/L of theoretical value
Temperature
NIST-traceable value (with correction factors)
Verification over range of sample values
Turbidity
0.1-10 NTU: + 10% of the calibration standard
11-40 NTU: + 8% of the calibration standard
41-100 NTU: + 6.5% of the calibration standard
> 100 NTU: + 5% of the calibration standard
Total Residual Chlorine
0.995 calibration curve correlation coeffecient
+ 10% of primary calibration standard value
+ 10% of secondary standard value
eNewsletter (automatic updates on QA topics & training)
http://www.dep.state.fl.us/labs/training/listserve.htm
Environmental Assessment Section
2600 Blair Stone Road MS 6511
Tallahassee, FL 32399-2400
SC 205 8065
(850) 245-8065
Contacts: [email protected]
Russel Frydenborg, Administrator
Silky Labie
Michael Blizzard
Thomas Deck
Denise Miller
Thomas Frick
Andrew Tintle
Jessica Patronis
Joyce Ziesenis