Field Sampling Considerations A Laboratory Perspective Joe Shaulys Sr. Account Executive

1. Field Sampling Considerations A Laboratory Perspective Joe Shaulys Sr. Account Executive

2. Agenda Definitions Test Method Selection Ordering Containers Chain of Custody Temperature Cooler Packing Hold-times What Happens at the Lab Upon Sample Receipt Questions

3. Definition of Terms Hold time – the elapsed time from sample collection by field personnel until its processing/analysis by lab personnel. Holding time requirements are dictated by the method. Grab Sample Composite Sample

4. Trip Blank - filled sample container, free of contaminants, transported to the site and returned to the laboratory unopened. Checks for VOC contamination originating from site conditions and sample shipment transport. Field Blank - contaminant-free “sample” transferred from one container to another at the site with appropriate preservative added. Checks reagent and environmental site contamination. Definition of Terms

5. Definition of Terms Duplicate Samples - two separate samples taken from the same source and analyzed independently. Evaluates precision of measurements throughout the analytical process. Matrix – the predominant material that comprises a sample, for example sludge. Matrix is not synonymous with phase (liquid or solid).

6. Method Selection Factors Regulatory requirements Permit specifications Data confidence requirements - qualitative and quantitative Time and cost

7. Environmental Regulatory Programs Clean Air Act (CAA) Clean Water Act (CWA) Safe Drinking Water Act (SDWA) Resource Conservation and Recovery Act (RCRA) Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) Superfund Amendments Reauthorization Act (SARA)

8. Method Sources For Analysis of Water, Soil and Wastes • EPA 600 Series Methods for Wastewater - CWA • EPA 500 Series Methods for Drinking Water - SDWA • EPA SW-846 for “Solid Wastes” - RCRA • Contract Lab Program (CLP) Methods - SARA & CERCLA • Standard Methods – SDWA & CWA • State Specific Methods – • Ex. NJ TPH, NJ LL TO-15

9. Method Sources For Analysis of Water, Soil and Wastes Same Analysis – Different Method – Different Compound Lists • Volatile Organic Compounds (VOCs) • BTEX (VOAs) – subset of VOCs • Halogens (VOHs) – subset of VOCs • Full VOCs – VOAs and VOHs • 624 – CWA • 524.2 - SDWA • 8260 – RCRA • CLP VOAs – CERCLA /SARA • 6210 – Standard Methods

10. Ordering Sample Containers Order by project, based on project description Number and types of containers Volume(s) of samples Determine how and when to deliver Review all requirements with Project Manager Preservatives and hold times Try to avoid over ordering. Bottles cannot be reused and preservatives have a shelf life

11. Example from analytical guide

12. Collecting the Samples • General Guidelines • Prevent contamination • Collect a representative sample: must reflect the nature of the site being characterized • Proper handling and preservatives

13. Proper Sample Collection – VOAs in Liquid • Collect at least 2 vials per sampling location • Fill the VOA vial TO THE RIM to avoid headspace • Invert vial and check for headspace. Total headspace should be no larger than a 3mm bubble (roughly the size of a small pea)

14. Sample Collection Vial containing headspace - Avoid this!

15. Proper Sample Collection – VOAs in Soil • EPA Method 5035 • A method for collection, preservation and preparation of soils for volatiles analysis • Originally introduced by EPA Dec.1996 • Approved by NYS-DOH ELAP for use on projects originating in New York • Benefits • Improves the capture and detection of volatiles • Minimizes loss of volatiles by preservation or collection without head-space • Minimizes the introduction of contamination • Samples can be analyzed directly from vials • Eliminates negative bias

16. Field Collection – Terracore

17. Field Collection – Terracore Using the plastic coring device, collect 5 grams of sample into a 40ml vial containing sodium bisulfate or DI water and a stir bar All samples must be collected in duplicate An additional 5 gram aliquot must be put in a 40ml vial containing 5 ml methanol (high concentration) An additional 100 gram jar unpreserved is collected for %moisture The lab will reweigh the pre-tared containers to calculate the actual sample weight Holding time is 14 days from collection for Bisulfate-preserved samples Samples collected with DI water vials must be received at the lab for analysis or freezing within 48 hrs of collection

18. Terracore Sampling Instructions Field Collection Options 1

19. Field Collection – Encore At minimum, 2 Encore samplers for direct collection of material for low level and 1 encore for high level analysis = 3 Encores An additional 2 oz soil jar for %moisture and screening Samples must be put in preservative within 48hr of collection Easy in the field- no weighing, no preservation Expensive for collection

20. Encore Sampling Instructions

21. Sample Collection Tips • TerraCore • Make sure the water or methanol layer covers the soil plug (should be 1:1 ratio of soil to water/methanol) • Don’t spill water or methanol preservative, this weight is accounted for in the tare weight. Redo if necessary • Make sure to wipe the VOA vial threads before capping. • Chill and make sure to get samples to the lab within 48 hrs if using DI water preserved vials. • Don’t add an additional label, this interferes with auto-sampler and adds un-accounted to tare weight to the vial. • Encore • Make sure to wipe the tip of the sampler and avoid getting soil in the o-ring mating surface

22. NYS DEC • NYS DEC acknowledges 5035 sampling but does not require it for all instances/sites • NYS DEC is not currently rejecting VOC analysis performed on samples received in soil jars and is accepting narrated/qualified data

23. Chain of Custody

24. Completing the Chain Of Custody • Your company and report-to info • Sample identification • Date, type, and time of sample collection • Record number of samples containers, preservation, and analyses • Signatures and dates of time of each person taking custody of samples

25. Completing the Chain Of Custody • “Analysis required by Method:” • Must be very specific – this will be the only written information the lab will have to log samples into the lab • There are multiple methods for some compounds •  Do not just put “Volatiles” on COC • If a limited list is needed, must be on COC • Ex. 8260 BTEX - lab will only report BTEX compounds not the whole list

26. Required Temperature Sample temperature must be kept within the required temperature range of 4C +/- 2C as per regulatory agency mandates to preserve sample integrity.

27. Packing the Cooler • Packing material will be supplied by the lab. Do not throw away upon receipt. • Avoid using packing material that absorbs water. • Bubble wrap, bubble wrap, bubble wrap… provides shock protection, thermal insulation. • Seal each container in bubble wrap, foam inserts or ziploc bags to keep labels from falling off. • Place shipping papers and COC in the cooler in a sealed ziploc bag.

28. Packing the Cooler • Keep on ice – natural is better • Tape cooler shut • Affix custody seals on cooler, if necessary • If coolers not being picked up by local courier, ship by fastest means possible • Use permanent ink on labels • 20 - 25 pound bag of ice per 48 quart cooler

29. Sample Transportation & Hold Times • Fecal Coliform – 6 hours • Hexavalent Chromium – 24 hours • Odor – 24 hours • Total Coliform – 30 hours • BOD – 48 hours • Chlorophyll A – 48 hours • Surfactants – 48 hours • Turbidity – 48 hours • Orthophosphorus – 48 hours • Nitrate & Nitrite – 48 hours • Coordinate, coordinate, coordinate

30. Sample Receipt at the Lab

31. Sample Receipt at the Lab

32. Common Questions • Why do we have to keep samples at 4C? • It is a required part of the preservation step required by the EPA methods for Organics to help minimize the loss of volatile and semi-volatile compounds. • Why does a lab prefer to have historical data on a particular sampling point? • Historical results allow the analyst to appropriately dilute samples on the first run to get compounds within the linear range of the instrument. Prevents carry over and major clean up which can delay project.

33. Thank you! Joe Shaulys Sr. Account Executive Pace Analytical Services 575 Broad Hollow Rd Melville, NY Questions?