Basic Sampling Procedures Quality Assurance FIPA Workshop Back

Basic Sampling Procedures & Quality Assurance FIPA Workshop Back to Basics West Palm Beach April 25, 2008

This presentation will…. • Help you navigate and use the DEP SOPs to your advantage. • Give you an opportunity to expand on what you already know and ask questions. • Provide basic field quality assurance practices to enhance field sampling experience.

General Sampling Considerations • Understanding of sampling and Data Quality Objectives • Obtaining a representative sample • Maintaining the integrity of the sample • Proper sampling protocols • Documentation

DEP QA Rule (FAC 62 -160) requires • Use DEP SOPs (revision date 2/1/04) – NEW DRAFT SOPS available on-line • Pre-approve alternative procedures • Keep mandatory documentation • Follow preservation & holding times • Auditing • DEP Data Reporting & Usability Criteria

The FDEP SOPs are a valuable resource • Quick reference • Clarify methods • Example forms • Tables ! The SOPs are currently undergoing revision !

DEP-SOP-001/01 Revision (2/1/04) DEP SOP Structure Naming Conventions – – FA FC FD FM Administrative & Quality Systems – FQ Field Cleaning – FS Documentation – FT Mobilization & Laboratory Quality Control Sampling Procedures Field Testing

SOP key Elements to a sampling program • Quality Manual (FA 3000) • Documentation (FD 1000) • Cleaning Procedures (FC 1000) • Field Quality Control (FQ 1000) • FT 1000 – FT 3000 Field Testing • General Sampling Procedures (FS 1000)

Good Documentation Habits “If it’s not documented, you didn’t do it!” “When in doubt, write it!”

Where to Find the SOPs: e. Newsletter http: //www. dep. state. fl. us/labs/training/listser ve. htm www. dep. state. fl. us/labs/sop/index

Quality Manual (FA 3000) Includes quality assurance policies and procedures for your specific organization

Field Quality Control (FQ 1000) Required Sampling QC Blanks – Optional – Duplicates or Replicates – Split Samples Blanks are not required for Microbiological, Toxicity, Field Parameters, Radon, BOD sampling

Why use blanks? • Show that samples have not been contaminated • Ensure that samples are representative of the sampling source • Field-collected data have stated limits of precision and accuracy

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

Equipment Blanks (FQ 1210) Analyte-free water collected by rinsing the sampling equipment at the sampling site. • Pre-cleaned equipment blank – Collect before using pre-cleaned equipment • Field-cleaned equipment blank – Collect after cleaning equipment in the field, in between sampling sites

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

• For each Project and each matrix and analyte combination (except VOCs), Collect 1 blank for 20 environmental samples (5% of samples) • Handle blanks exactly like the associated environmental samples!

Field Testing

FT 1000 – FT 3000 Field Testing • p. H • Specific • • Conductance Temperature Dissolved Oxygen Turbidity Residual Chlorine

Field Testing (FT 1000 – FT 3000) Collecting data in the field • Calibration of instruments • Verification of instruments • Documentation

Table FT 1000 -1 Field Testing

General Sampling Procedures (FS 1000) Important information for all types of sampling Useful tables: – Sample Preservation, Holding Times & Container Types – Construction Materials & Approved Sampling Equipment

FS 2110 & FS 2430 Grab Sampling Equipment selection depends on project objectives and analyte groups…. Depth Sampler Composite Other Intermediate Devices Pump and tubing

General Aqueous Sampling (FS 2000) • Collection, Filtration and Preservation Procedures • Instructions for Specific Analyte Groups

FS 2000 & FS 2001 Filtering erformed on-site P Before chemical preservation &Preservation Use tables FS 1000 -4 through FS 1000 -8

Frequency of p. H Checks • Verify all p. H-Preserved Samples – Check one sample per analyte group • • Monthly Sampling – check quarterly Weekly Sampling– check monthly Daily Sampling– check weekly Other Sampling frequencies – First sampling event – check all samples – Subsequent visits – one sample per analyte group • On-Site p. H Checks Not Required for VOCs

What Do I Need to Know when Sampling for Volatile Organics? • Collect the correct number of vials • • • required by lab No head space – Discard sample if combined diameter of all bubbles is greater than 5 mm – DO NOT reopen to additional sample! Dechlorination agent must be in vial before sample is added (if applicable) Add acid (if necessary) prior to filling to convex meniscus Cool with wet ice Trip blanks are required

What Do I Need to Know about Sampling for Oil & Grease and TRPHs? • 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 Wet Ice

What Do I Need to Know about Sampling for Microbiologicals? • Collect Last (Short Holding Time) • Sterilized Containers Required • Use Dechlorinating Agent (if • • Applicable) Thoroughly Rinse any Intermediate Devices Don’t Underfill or Overfill Whirlpaks Close Whirlpaks Securely Cool with Wet Ice

What Do I Need to Know about Sampling for Metals? • No Acid for Samples Analyzed for Chromium VI • Preserve with Nitric Acid (HNO 3) at least 24 hours prior to analysis immediate preservation is no longer required (except boron and mercury)

Wastewater Sampling (FS 2400)

FS 2100 & FS 2400 Sampling Strategies for Surface Water and Wastewater Locations • Collect – Least to most contaminated • Downstream to upstream • Bow of the boat – Upwind away from fuel sources – Upstream and away from body – 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 2110, FS 2420 & FS 2430 Grab Samples Discrete sample collected over a period of time not exceeding 15 minutes Indicated uses: • Snapshot in time • Direct observation of conditions at • • time of sampling Intermittent flows Constant waste stream or waterbody 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 Collect Grabs for: • • • Cyanide Oil and Grease Residual Chlorine p. H VOC TRPH • Sulfides and H 2 S • FL-PRO • Dissolved oxygen • Dissolved analytes • Bacteria • Specific conductance

Automatic Samplers (FS 2400) • Composite sampling vs. discrete • Flow-proportional sampling • Time composite sampling

FS 2110, FS 2423 & FS 2430 Composite Sample. A sample collected over time, • • taken either by continuous sampling or by mixing discrete Indicated uses: samples. Composite samples Continuous flow reflect the average Limited analytical capacity characteristics during the Average analyte concentration over compositing period 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 2423 Composite Types • Time – Sub-sample aliquots collected at recurring interval – Flow variation no more than ± 10% of average flow • Flow proportional • • – Equal sample volumes collected at time intervals proportional to flow – Adjusted sample volumes collected proportional to flow at constant collection time interval Sequential Continuous Areal Manual or automated – Ice or refrigeration for unattended sampling

FS 2100 & 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

BIOSOLIDS • • Domestic Wastewater Sludges Industrial Wastewater Sludges of Variable Composition Samples for Metals Must Be Composites Samples for Pathogens and Volatile Solids Must Be Grabs

Biosolids Sampling Considerations • Safety Precautions • • • – Standard methods 1060 Infectious Waste Transport – Interstate shipment of >4 liters prohibited – Filter infectious samples in the field Equipment Types and Material construction Container Types

Biosolids Safety Precautions • • • Follow Procedures Outlined in SM 1060 Wear Gloves and Change as Needed Clean Sample Container Exteriors before Delivering Samples to Others Take Precautions Not to Touch Other Areas of the Body While Sampling Keep Inoculations up to Date Monitor Enclosed Sampling Areas for Dangerous Gases

Cryptosporidium and Giardia Wastewater Sampling (FS 2450) • Use EPA method 1623 • Follow bacteriological sampling restrictions in FS 2005

Documentation (FD 1000) • There are universal requirements as well as specifics for each type of documentation. – Example forms

Documentation (FD 1000) • Unique identification of sample containers • 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

Documentation (FD 1000) • • • 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

Documenting Sample Information • Link bottles to records. • Unique bottle ID • Also, – Site – Date – Time – Numbered if multiples

Contacts: firstname. lastname@dep. state. fl. us Silky Labie Andrew Tintle Denise Miller Russel Frydenborg, Administrator

Will DEP Accept My DATA? Your Goal: Ensure that the Results Accurately Represent the Sample Source Bottom Line