Basic Sampling Procedures & Quality Assurance

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. • 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.

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

4. 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

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

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

7. SOP key Elements to a sampling program • Quality Manual (FA3000) • Documentation (FD 1000) • Cleaning Procedures (FC 1000) • Field Quality Control (FQ 1000) • FT 1000 – FT 3000 Field Testing • 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/listserve.htm www.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 • Ensure that samples are representative of the sampling source • 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 • Collect before using pre-cleaned equipment • 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. • 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) • Handle blanks exactly like the associated environmental samples!

17. Field Testing

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

19. Field Testing (FT 1000 – FT 3000) Collecting data in the field • Calibration of instruments • Verification of instruments • 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. FS 2110 & FS 2430 Grab Sampling Depth Sampler Equipment selection depends on project objectives and analyte groups…. Composite Pump and tubing Other Intermediate Devices

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

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

25. Frequency of pH Checks • Verify all pH-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 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 • 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) • Add acid (if necessary) prior to filling to convex meniscus • Cool with wet ice • 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 Pre-Rinse Bottles With Sample • Do Not use Automatic Samplers • 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) • 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

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

30. Wastewater Sampling (FS2400)

31. 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 and 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

32. 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 Grab Samples

33. Cyanide Oil and Grease Residual Chlorine pH VOC TRPH Sulfides and H2S FL-PRO Dissolved oxygen Dissolved analytes Bacteria Specific conductance FS 2110, FS 2420 & FS 2430 Collect Grabs for:

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

35. 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 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 Composite Sample

36. 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

37. 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

38. 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

39. BiosolidsSampling 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

40. BiosolidsSafety 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

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

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

43. 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

44. 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

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

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

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