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Field Sampling Considerations A Laboratory Perspective Joe Shaulys Sr. Account Executive. Agenda. Definitions Test Method Selection Ordering Containers Chain of Custody Temperature Cooler Packing Hold-times What Happens at the Lab Upon Sample Receipt Questions. Definition of Terms.

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Field Sampling Considerations

A Laboratory Perspective

Joe Shaulys

Sr. Account Executive



Test Method Selection

Ordering Containers

Chain of Custody


Cooler Packing


What Happens at the Lab Upon Sample Receipt


definition of terms
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

definition of terms1
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
definition of terms2
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).

method selection factors
Method Selection Factors

Regulatory requirements

Permit specifications

Data confidence requirements - qualitative and quantitative

Time and cost

environmental regulatory programs
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)

method sources for analysis of water soil and wastes
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
method sources for analysis of water soil and wastes1
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
  • 6210 – Standard Methods
ordering sample containers
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

collecting the samples
Collecting the Samples
  • General Guidelines
    • Prevent contamination
    • Collect a representative sample: must reflect the nature of the site being characterized
    • Proper handling and preservatives
proper sample collection voas in liquid
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)
sample collection
Sample Collection

Vial containing headspace - Avoid this!

proper sample collection voas in soil
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
field collection terracore1
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

terracore sampling instructions
Terracore Sampling Instructions

Field Collection Options 1

field collection encore
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

sample collection tips
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
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
completing the chain of custody
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
completing the chain of custody1
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
required temperature
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.

packing the cooler
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.
packing the cooler1
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
sample transportation hold times
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
common questions
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.
Thank you!

Joe Shaulys

Sr. Account Executive

Pace Analytical Services

575 Broad Hollow Rd

Melville, NY