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

2. This presentation will…. Help you navigate and use the DEP SOPs to your advantage. 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. 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. Provide basic field quality assurance practices to enhance field sampling experience.

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

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

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

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

7. SOP key Elements to a sampling program Quality Manual (FA3000) Quality Manual (FA3000) Documentation (FD 1000) Documentation (FD 1000) Cleaning Procedures (FC 1000) Cleaning Procedures (FC 1000) Field Quality Control (FQ 1000) Field Quality Control (FQ 1000) FT 1000 – FT 3000 Field Testing FT 1000 – FT 3000 Field Testing General Sampling Procedures (FS 1000) General Sampling Procedures (FS 1000)

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

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

10. Quality Manual (FA3000) Includes quality assurance policies and procedures for your specific organization

11. 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

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

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

14. Equipment Blanks (FQ1210) Analyte-free water collected by rinsing the sampling equipment at the sampling site. Pre-cleaned equipment blank Pre-cleaned equipment blank – Collect before using pre-cleaned equipment Field-cleaned equipment blank Field-cleaned equipment blank – Collect after cleaning equipment in the field, in between sampling sites

15. Trip Blanks (VOCs Only) VOC vials filled with analyte-free water accompany the real VOC samples through the entire sampling trip. 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.

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

17. Field Testing

18. FT 1000 – FT 3000 Field Testing pH pH Specific Conductance Specific Conductance Temperature Temperature Dissolved Oxygen Dissolved Oxygen Turbidity Turbidity Residual Chlorine Residual Chlorine

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

20. Table FT 1000-1 Field Testing

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

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

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

24. Preservation  Use tables FS 1000-4 through FS 1000-8 FS 2000 & FS 2001Filtering &  Performed on-site  Before chemical preservation

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

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

27. 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 Skim Surface of Water (Unless Required by Sampling Plan) Do Not Pre-Rinse Bottles With Sample Do Not Pre-Rinse Bottles With Sample Do Not use Automatic Samplers Do Not use Automatic Samplers Preserve with Sulfuric or Hydrochloric Acid and Wet Ice Preserve with Sulfuric or Hydrochloric Acid and Wet Ice

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

29. What Do I Need to Know about Sampling for Metals? No Acid for Samples Analyzed for Chromium VI No Acid for Samples Analyzed for Chromium VI Preserve with Nitric Acid (HNO3) at least 24 hours prior to analysis immediate preservation is no longer required (except boron and mercury) Preserve with Nitric Acid (HNO3) at least 24 hours prior to analysis immediate preservation is no longer required (except boron and mercury)

30. Wastewater Sampling (FS2400)

31. Sampling Strategies for Surface Water and Wastewater Locations Collect Collect –Least to most contaminated Downstream to upstream Downstream to upstream Bow of the boat Bow of the boat –Upwind and away from fuel sources –Upstream and away from body –Sample water before collecting sediments Consider: 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

32. Grab Samples Grab Samples Discrete sample collected over a period of time not exceeding 15 minutes Indicated uses: Snapshot in time Snapshot in time Direct observation of conditions at time of sampling Direct observation of conditions at time of sampling Intermittent flows Intermittent flows Constant waste stream or waterbody characteristics Constant waste stream or waterbody characteristics Batch discharges Batch discharges Determining min/max concentrations Determining min/max concentrations Tracing slug loads or spills Tracing slug loads or spills Analytes with short holding times Analytes with short holding times Analytes altered by composite techniques Analytes altered by composite techniques FS 2110, FS 2420 & FS 2430

33. Collect Grabs for: Cyanide Cyanide Oil and Grease Oil and Grease Residual Chlorine Residual Chlorine pH pH VOC VOC TRPH TRPH Sulfides and H 2 S Sulfides and H 2 S FL-PRO FL-PRO Dissolved oxygen Dissolved oxygen Dissolved analytes Dissolved analytes Bacteria Bacteria Specific conductance Specific conductance FS 2110, FS 2420 & FS 2430

34. Automatic Samplers (FS2400) Composite sampling vs. discrete Flow-proportional sampling Time composite sampling

35. 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 Indicated uses: Continuous flow Continuous flow Limited analytical capacity Limited analytical capacity Average analyte concentration over time Average analyte concentration over time Calculating mass/unit time loadings Calculating mass/unit time loadings Correlation of concentration data with flow Correlation of concentration data with flow Reduction of sampling errors and hazard exposure with use of autosamplers Reduction of sampling errors and hazard exposure with use of autosamplers Unattended sampling with autosamplers Unattended sampling with autosamplers FS 2110, FS 2410, FS 2423 & FS 2430

36. Composite Types Time Time –Sub-sample aliquots collected at recurring interval –Flow variation no more than ± 10% of average flow Flow proportional 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 Sequential Continuous Continuous Areal Areal Manual or automated Manual or automated –Ice or refrigeration for unattended sampling FS 2423

37. Representative Sampling and Contamination Prevention Mix discrete sub-samples thoroughly prior to manual compositing Mix discrete sub-samples thoroughly prior to manual compositing Avoid cross-contamination between sampling points Avoid cross-contamination between sampling points Clean reusable equipment appropriately Clean reusable equipment appropriately Collect field QC blanks as applicable Collect field QC blanks as applicable Flush wastewater taps to remove settled solids and reduce flow before sampling Flush wastewater taps to remove settled solids and reduce flow before sampling Dechlorinate wastewater samples when required Dechlorinate wastewater samples when required –VOCs, extractable organics, microbiology, cyanide FS 2100 & 2400

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

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

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

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

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

43. Documentation (FD 1000) Unique identification of sample containers Unique identification of sample containers Number of sample containers for each unique container identification Number of sample containers for each unique container identification Site and sampling point identification and matrix Site and sampling point identification and matrix Sample type (grab, composite, equipment blank, trip blank, etc.) Sample type (grab, composite, equipment blank, trip blank, etc.) Sampler names, initials or signatures Sampler names, initials or signatures Sample collection date, time, depth, flow rate Sample collection date, time, depth, flow rate Sample preservation and preservation checks Sample preservation and preservation checks Notes about sample problems Notes about sample problems

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

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

46. DeniseMiller AndrewTintle SilkyLabie Contacts: firstname.lastname@dep.state.fl.us RusselFrydenborg,Administrator

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