Basic Sampling Basic Sampling ProceduresProcedures

& Quality Assurance & Quality Assurance

FIPA WorkshopFIPA WorkshopBack to BasicsBack to Basics

West Palm Beach West Palm Beach April 25, 2008April 25, 2008

This presentation will….This presentation will….

• Help you navigate and use the Help you navigate and use the DEP SOPs to your advantage.DEP SOPs to your advantage.

• Give you an opportunity to Give you an opportunity to expand on what you already know expand on what you already know and ask questions.and ask questions.

• Provide basic field quality Provide basic field quality assurance practices to enhance assurance practices to enhance field sampling experience.field sampling experience.

General Sampling General Sampling ConsiderationsConsiderations

• Understanding of sampling and Understanding of sampling and Data Quality ObjectivesData Quality Objectives

• Obtaining a representative sampleObtaining a representative sample

• Maintaining the integrity of the Maintaining the integrity of the samplesample

• Proper sampling protocolsProper sampling protocols

• DocumentationDocumentation

DEP QA Rule (FAC 62-160) DEP QA Rule (FAC 62-160) requiresrequires

• Use DEP SOPs (revision date Use DEP SOPs (revision date 2/1/04)2/1/04)– NEW DRAFT SOPS available on-lineNEW DRAFT SOPS available on-line

• Pre-approve alternative proceduresPre-approve alternative procedures• Keep mandatory documentationKeep mandatory documentation• Follow preservation & holding Follow preservation & holding

timestimes• AuditingAuditing• DEP Data Reporting & Usability DEP Data Reporting & Usability

CriteriaCriteria

The FDEP SOPs are a valuable The FDEP SOPs are a valuable resourceresource

• Quick referenceQuick reference

• Clarify methodsClarify methods

• Example formsExample forms

• TablesTables

! The SOPs are currently undergoing revision !

DEP SOPDEP SOPStructureStructure

Naming ConventionsNaming Conventions– FA Administrative & Quality FA Administrative & Quality

SystemsSystems– FC Field CleaningFC Field Cleaning– FD DocumentationFD Documentation– FM Mobilization & Laboratory FM Mobilization & Laboratory

1000General Sampling

3000Soil

4000Sediment

5000Waste

6000Biological Tissue

7000Biological Community

8000Miscellaneous

FSField Sampling

2000Aqueous

2000General Aqueous

2200Groundwater

2300Potable Water

2400Wastewater

2500Stormwater

FSField Sampling

2000Aqueous

2100Surface Water

2100Surface Water

General

2110Grab Samples

2120Composite

2130Water Depth Grab

2140W.D. Composite

– FQ Quality ControlFQ Quality Control– FS Sampling ProceduresFS Sampling Procedures– FT Field TestingFT Field Testing

DEP-SOP-001/01Revision (2/1/04)

SOP key Elements to a SOP key Elements to a sampling programsampling program

• Quality Manual Quality Manual (FA3000)(FA3000)

• Documentation (Documentation (FD 1000)FD 1000)

• Cleaning Procedures Cleaning Procedures (FC 1000)(FC 1000)

• Field Quality Control (FQ 1000) Field Quality Control (FQ 1000)

• FT 1000 – FT 3000 Field TestingFT 1000 – FT 3000 Field Testing

• General Sampling Procedures (FS General Sampling Procedures (FS 1000)1000)

Good Documentation Good Documentation HabitsHabits

“If it’s not documented, you didn’t do it!”

“When in doubt, write it!”

Where to Find the SOPs:Where to Find the SOPs:

eNewslettereNewsletterhttp://www.dep.state.fl.us/labs/training/listserve.http://www.dep.state.fl.us/labs/training/listserve.htmhtm

www.dep.state.fl.us/labs/sop/www.dep.state.fl.us/labs/sop/indexindex

Quality Manual Quality Manual (FA3000)(FA3000)

Includes quality assurance policies and procedures for your

specific organization

Field Quality Control Field Quality Control ((FQ 1000)FQ 1000)

RequiredRequiredSampling QC BlanksSampling QC Blanks

– OptionalOptional

– Duplicates or ReplicatesDuplicates or Replicates– Split SamplesSplit Samples

Blanks are not required for Microbiological, Toxicity, Field Blanks are not required for Microbiological, Toxicity, Field Parameters, Radon, BOD samplingParameters, Radon, BOD sampling

Why use blanks?Why use blanks?

• Show that samples have not Show that samples have not been contaminatedbeen contaminated

• Ensure that samples are Ensure that samples are representative of the sampling representative of the sampling sourcesource

• Field-collected data have stated Field-collected data have stated limits of precision and accuracylimits of precision and accuracy

Field BlanksField Blanks

Analyte-free water collected Analyte-free water collected directly into a sample bottle at directly into a sample bottle at the sampling site.the sampling site.

Equipment Blanks Equipment Blanks (FQ1210)(FQ1210)

Analyte-free water collected by rinsing the Analyte-free water collected by rinsing the sampling equipment at the sampling site.sampling equipment at the sampling site.

•Pre-cleaned equipment blankPre-cleaned equipment blank– Collect before using pre-cleaned equipmentCollect before using pre-cleaned equipment

•Field-cleaned equipment blankField-cleaned equipment blank– Collect after cleaning equipment in the field, Collect after cleaning equipment in the field, in between sampling sitesin between sampling sites

Trip Blanks (VOCs Trip Blanks (VOCs Only)Only)

• VOC vials filled with analyte-free VOC vials filled with analyte-free water accompany the real VOC water accompany the real VOC samples through the entire samples through the entire sampling trip.sampling trip.– Remain unopened until analysisRemain unopened until analysis– Min. 1 vial per VOC cooler, and trip.Min. 1 vial per VOC cooler, and trip.

• For each Project and each matrix For each Project and each matrix and analyte combination (except and analyte combination (except VOCs), Collect 1 blank for 20 VOCs), Collect 1 blank for 20 environmental samples (5% of environmental samples (5% of samples)samples)

• Handle blanks exactly like the Handle blanks exactly like the associated environmental samples!associated environmental samples!

Field TestingField Testing

FT 1000 – FT 3000 FT 1000 – FT 3000 Field TestingField Testing

• pHpH

• Specific Specific ConductanceConductance

• TemperatureTemperature

• Dissolved Dissolved OxygenOxygen

• TurbidityTurbidity

• Residual Residual ChlorineChlorine

Field Testing Field Testing (FT 1000 – FT 3000)(FT 1000 – FT 3000)

Collecting data in the fieldCollecting data in the field

• Calibration of instrumentsCalibration of instruments

• Verification of instrumentsVerification of instruments

• DocumentationDocumentation

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

Table FT 1000-1 Field Testing

General Sampling Procedures General Sampling Procedures ((FS 1000)FS 1000)

Useful tables:Useful tables:– Sample Preservation, Holding Times & Sample Preservation, Holding Times &

Container TypesContainer Types– Construction Materials & Approved Construction Materials & Approved

Sampling EquipmentSampling Equipment

Important information for all types of sampling

Equipment selection depends on project Equipment selection depends on project objectives and analyte groups….objectives and analyte groups….

FS 2110 & FS 2430 Grab Sampling

Depth Depth SamplerSampler

Pump and tubingPump and tubing

CompositCompositee

Other Intermediate Other Intermediate DevicesDevices

General Aqueous General Aqueous SamplingSampling(FS 2000)(FS 2000)

• Collection, Filtration and Collection, Filtration and Preservation ProceduresPreservation Procedures

• Instructions for Specific Analyte Instructions for Specific Analyte GroupsGroups

PreservationPreservationUse tables FS 1000-4 through FS 1000-8Use tables FS 1000-4 through FS 1000-8

FS 2000 & FS 2001FilterinFilteringg

&

Performed on-siteBefore chemical preservation

Frequency of pH ChecksFrequency of pH Checks

• Verify all pH-Preserved SamplesVerify all pH-Preserved Samples – Check one sample per analyte groupCheck one sample per analyte group

• Monthly Sampling – check quarterlyMonthly Sampling – check quarterly

• Weekly Sampling– check monthlyWeekly Sampling– check monthly

• Daily Sampling– check weeklyDaily Sampling– check weekly

• Other Sampling frequenciesOther Sampling frequencies

– First sampling event – check First sampling event – check allall samples samples– Subsequent visits – one sample per analyte Subsequent visits – one sample per analyte

groupgroup

• On-Site pH Checks Not Required for VOCsOn-Site pH Checks Not Required for VOCs

What Do I Need to Know What Do I Need to Know when Sampling for Volatile when Sampling for Volatile

Organics?Organics?• Collect the correct number of vials Collect the correct number of vials

required by labrequired by lab• No head spaceNo head space

– Discard sample if combined Discard sample if combined diameter of all bubbles is diameter of all bubbles is greater than 5 mmgreater than 5 mm

– DO NOT reopen to add DO NOT reopen to add additional sample!additional sample!

• Dechlorination agent must be in Dechlorination agent must be in vial vial beforebefore sample is added (if sample is added (if applicable)applicable)

• Add acid (if necessary) prior to Add acid (if necessary) prior to filling to convex meniscusfilling to convex meniscus

• Cool with wet iceCool with wet ice• Trip blanks are requiredTrip blanks are required

What Do I Need to Know about What Do I Need to Know about Sampling for Oil & Grease and Sampling for Oil & Grease and

TRPHs?TRPHs?• Do Not Skim Surface of Water (Unless Do Not Skim Surface of Water (Unless

Required by Sampling Plan)Required by Sampling Plan)

• Do Not Pre-Rinse Bottles With SampleDo Not Pre-Rinse Bottles With Sample

• Do Not use Automatic SamplersDo Not use Automatic Samplers

• Preserve with Sulfuric or Hydrochloric Acid Preserve with Sulfuric or Hydrochloric Acid andand Wet IceWet Ice

What Do I Need to Know What Do I Need to Know about Sampling for about Sampling for Microbiologicals?Microbiologicals?

• Collect Last (Short Holding Collect Last (Short Holding Time)Time)

• Sterilized Containers RequiredSterilized Containers Required• Use Dechlorinating Agent (if Use Dechlorinating Agent (if

Applicable)Applicable)• Thoroughly Rinse any Thoroughly Rinse any

Intermediate DevicesIntermediate Devices• Don’t Underfill or Overfill Don’t Underfill or Overfill

WhirlpaksWhirlpaks• Close Whirlpaks SecurelyClose Whirlpaks Securely• Cool with Wet IceCool with Wet Ice

What Do I Need to Know What Do I Need to Know about Sampling for about Sampling for

Metals?Metals?• No Acid for Samples Analyzed for Chromium VINo Acid for Samples Analyzed for Chromium VI

• Preserve with Nitric Acid (HNO3) Preserve with Nitric Acid (HNO3) at least 24 at least 24 hours prior to analysishours prior to analysis immediate preservation immediate preservation is no longer required (except boron and is no longer required (except boron and mercury)mercury)

Wastewater Sampling Wastewater Sampling (FS2400)(FS2400)

Sampling Strategies for Surface Sampling Strategies for Surface Water and Wastewater LocationsWater and Wastewater Locations

• Collect Collect – Least to most contaminatedLeast to most contaminated

•Downstream to upstreamDownstream to upstream•Bow of the boatBow of the boat

– Upwind and away from fuel sourcesUpwind and away from fuel sources– Upstream and away from bodyUpstream and away from body– Sample water before collecting sedimentsSample water before collecting sediments

• Consider:Consider:– Location relative to artificial structuresLocation relative to artificial structures– Permit-specific sampling pointsPermit-specific sampling points– Flow characteristics of sample sourceFlow characteristics of sample source– Heterogeneity or homogeneity of sample Heterogeneity or homogeneity of sample

source source

FS 2100 & FS 2400

Grab Grab SamplesSamples

Discrete sample Discrete sample collected over a collected over a

period of time not period of time not exceeding 15 exceeding 15

minutes minutes

Indicated uses:Indicated uses:• Snapshot in time Snapshot in time • Direct observation of Direct observation of

conditions at time of samplingconditions at time of sampling• Intermittent flowsIntermittent flows• Constant waste stream or Constant waste stream or

waterbody characteristicswaterbody characteristics• Batch dischargesBatch discharges• Determining min/max Determining min/max

concentrationsconcentrations• Tracing slug loads or spillsTracing slug loads or spills• Analytes with short holding Analytes with short holding

timestimes• Analytes altered by composite Analytes altered by composite

techniquestechniques

FS 2110, FS 2420 & FS 2430

Collect Grabs for:Collect Grabs for:

• CyanideCyanide

• Oil and GreaseOil and Grease

• Residual ChlorineResidual Chlorine

• pHpH

• VOCVOC

• TRPHTRPH

• Sulfides and HSulfides and H22SS

• FL-PROFL-PRO

• Dissolved oxygenDissolved oxygen

• Dissolved analytesDissolved analytes

• BacteriaBacteria

• Specific Specific conductanceconductance

FS 2110, FS 2420 & FS 2430

Automatic Samplers Automatic Samplers (FS2400)(FS2400)

•Composite sampling vs. discrete •Flow-proportional sampling•Time composite sampling

Composite Composite SampleSample A sample collected over A sample collected over

time, taken either by time, taken either by continuous sampling or by continuous sampling or by mixing discrete samples. mixing discrete samples. Composite samples reflect Composite samples reflect the average the average characteristics during the characteristics during the compositing period compositing period

Indicated uses:Indicated uses:• Continuous flowContinuous flow• Limited analytical capacityLimited analytical capacity• Average analyte concentration Average analyte concentration

over timeover time• Calculating mass/unit time Calculating mass/unit time

loadingsloadings• Correlation of concentration Correlation of concentration

data with flowdata with flow• Reduction of sampling errors Reduction of sampling errors

and hazard exposure with use and hazard exposure with use of autosamplersof autosamplers

• Unattended sampling with Unattended sampling with autosamplersautosamplers

FS 2110, FS 2410, FS 2423 & FS 2430

Composite TypesComposite Types• TimeTime

– Sub-sample aliquots collected at recurring interval Sub-sample aliquots collected at recurring interval – Flow variation no more than Flow variation no more than ± 10% of average flow± 10% of average flow

• Flow proportionalFlow proportional– Equal sample volumes collected at time intervals Equal sample volumes collected at time intervals

proportional to flowproportional to flow– Adjusted sample volumes collected proportional to flow at Adjusted sample volumes collected proportional to flow at

constant collection time interval constant collection time interval • SequentialSequential• ContinuousContinuous• ArealAreal• Manual or automatedManual or automated

– Ice or refrigeration for unattended samplingIce or refrigeration for unattended sampling

FS 2423

Representative Sampling Representative Sampling and Contamination and Contamination Prevention Prevention

• Mix discrete sub-samples thoroughly prior to Mix discrete sub-samples thoroughly prior to manual compositingmanual compositing

• Avoid cross-contamination between sampling Avoid cross-contamination between sampling pointspoints

• Clean reusable equipment appropriatelyClean reusable equipment appropriately• Collect field QC blanks as applicableCollect field QC blanks as applicable• Flush wastewater taps to remove settled solids Flush wastewater taps to remove settled solids

and reduce flow before samplingand reduce flow before sampling• Dechlorinate wastewater samples when Dechlorinate wastewater samples when

requiredrequired– VOCs, extractable organics, microbiology, VOCs, extractable organics, microbiology,

cyanidecyanide

FS 2100 & 2400

BIOSOLIDSBIOSOLIDS• Domestic Wastewater SludgesDomestic Wastewater Sludges• Industrial Wastewater Sludges of Variable Industrial Wastewater Sludges of Variable

CompositionComposition• Samples for Metals Must Be CompositesSamples for Metals Must Be Composites• Samples for Pathogens and Volatile Solids Must Samples for Pathogens and Volatile Solids Must

Be GrabsBe Grabs

BiosolidsBiosolidsSampling ConsiderationsSampling Considerations

• Safety PrecautionsSafety Precautions– Standard methods 1060Standard methods 1060

• Infectious Waste TransportInfectious Waste Transport– Interstate shipment of >4 liters prohibitedInterstate shipment of >4 liters prohibited– Filter infectious samples in the fieldFilter infectious samples in the field

• Equipment Types and Material constructionEquipment Types and Material construction• Container TypesContainer Types

BiosolidsBiosolidsSafety PrecautionsSafety Precautions

• Follow Procedures Outlined in SM 1060Follow Procedures Outlined in SM 1060• Wear Gloves and Change as NeededWear Gloves and Change as Needed• Clean Sample Container Exteriors before Clean Sample Container Exteriors before

Delivering Samples to OthersDelivering Samples to Others• Take Precautions Not to Touch Other Areas of the Take Precautions Not to Touch Other Areas of the

Body While SamplingBody While Sampling• Keep Inoculations up to DateKeep Inoculations up to Date• Monitor Enclosed Sampling Areas for Dangerous Monitor Enclosed Sampling Areas for Dangerous

GasesGases

CryptosporidiumCryptosporidium and and GiardiaGiardia Wastewater Sampling Wastewater Sampling ((FS 2450)FS 2450)

• Use EPA method 1623Use EPA method 1623

• Follow bacteriological sampling Follow bacteriological sampling restrictions in FS 2005restrictions in FS 2005

Documentation Documentation ((FD 1000)FD 1000)

• There are universal requirements There are universal requirements as well as specifics for each type as well as specifics for each type of documentation.of documentation.– Example formsExample forms

Documentation Documentation ((FD 1000)FD 1000) • Unique identification of sample containers Unique identification of sample containers • Number of sample containers for each unique Number of sample containers for each unique

container identificationcontainer identification• Site and sampling point identification and Site and sampling point identification and

matrix matrix • Sample type (grab, composite, equipment Sample type (grab, composite, equipment

blank, trip blank, etc.)blank, trip blank, etc.)• Sampler names, initials or signaturesSampler names, initials or signatures• Sample collection date, time, depth, flow rateSample collection date, time, depth, flow rate• Sample preservation and preservation checksSample preservation and preservation checks• Notes about sample problemsNotes about sample problems

Documentation Documentation ((FD 1000)FD 1000) • Ambient field conditions Ambient field conditions • Monitor well purging and stabilization logMonitor well purging and stabilization log• Sampling and purging equipment usedSampling and purging equipment used• Equipment decontamination logEquipment decontamination log• Equipment maintenance logEquipment maintenance log• Field testing measurementsField testing measurements• Field meter calibration recordsField meter calibration records• Links with site maps, videos, photosLinks with site maps, videos, photos• Transmittal of samples to lab or other partyTransmittal of samples to lab or other party

Documenting Sample Documenting Sample InformationInformation

• Link bottles to records.Link bottles to records.

• Unique bottle IDUnique bottle ID

• Also, Also, – SiteSite– DateDate– Time Time – Numbered if multiplesNumbered if multiples

Denise Denise MillerMiller

AndrewAndrewTintleTintle

Silky Silky LabieLabie

Contacts: firstname.lastname@dep.state.fl.us

Russel Russel Frydenborg, Frydenborg, AdministratorAdministrator

Bottom Bottom LineLine

Will DEP Accept My DATA?Your Goal:

Ensure that the Results Accurately Represent the

Sample Source