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Water Sampling Kits from the Lab Perspective

Kevin Thoenen

Chemical Laboratory Manager

Environmental Services Program

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Sampling Kits & Challenges

  • We send many different kits with a wide variety of containers
    • Some look the same but have very different purposes
    • Some have very specific collection procedures
    • Some have collection requirements specific to locations in the water system

  • Instructions are included with every kit
    • Important to use the instruction sheet, read all additional information provided
    • If you have questions about collection, do not hesitate to contact us

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Sampling Kits & Challenges

  • Sample collection is the most critical step for the lab to provide good results
    • Your job is important, we appreciate your diligence and the work you do

  • Returning kits to the lab
    • Challenges with shipping company
    • Temperature requirements
    • Breakage

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Sampling Containers

  • Some contain liquid or powdered preservatives

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Common Contaminant Groups Monitored

  • Inorganic Compounds (IOCs)
  • Nitrate/Nitrite only
  • Volatile Organic Compounds (VOCs)
  • Synthetic Organic Compounds (SOCs)
  • Disinfection Byproducts (DBPs)
  • Lead and Copper (PbCu)

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Inorganic Compounds (IOCs)

  • Metals

– Clear Nalgene® 500 mL

  • Wet Chemistry (Minerals) Analytes
    • Clear Nalgene 500 mL
    • Chloride, Sulfate, Fluoride, Total Dissolved Solids

  • Possibly......
    • Cyanide (non-chlorinated systems) – amber Nalgene 60 mL
    • Nitrate-Nitrite – clear Nalgene 60 mL
    • Ammonia – clear Nalgene 60 mL

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IOC Containers

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Common Issues with IOC Kits

  • Temperature
    • Samples must be received at, or below, 6°C
      • Lab checks temperature upon receipt of samples
    • Large volume containers, ice packs alone will not cool the samples to 6°C
    • Refrigerate overnight prior to packing, freeze ice packs overnight (12 hours)
    • Ice bath (50% ice/water ratio), 15-20 minutes should bring temperature down

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Common Issues with IOC Kits

  • Nitrate, Cyanide, and Ammonia containers
    • Small amounts of liquid preservative to adjust the pH of the sample
    • Lab inspects the sample for proper preservation upon receipt
    • Do not rinse containers

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Nitrate/Nitrite

  • Single 60 ml clear Nalgene
  • Contains a small amount of preservative

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Volatile Organic Compounds (VOC)

  • Amber glass containers – two (2) - 40 mL
  • Include field blanks filled with water free of VOCs
    • All you have to do is return, do not open
  • Chlorinated water supply kits
    • Have an additional two (2) - 40 mL clear glass vials to de-chlorinate – contain a white granular material, sodium thiosulfate
      • Removes any free chlorine in the sample
    • Fill one clear vial, pour into the amber vial, return empty
      • Top off the amber vial with sample if necessary
    • Follow the same procedure with second vials

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Volatile Organic Compounds (VOC)

  • Amber vials have a small amount of liquid preservative
  • Do not rinse clear or amber vials

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Common Issues with VOC Kits

  • Too much headspace in the vials
  • Rinsing vials prior to sample collection
    • Analysts check for preservation
    • pH unacceptable
  • Chlorinated Supplies, clear vials not used properly
    • Not used at all
    • Come back filled with sample, instructions say to return empty
      • Fill clear vial and pour into one amber vial, only one use

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Common Issues with VOC Kits

  • Temperature – must be received at, or below, 6°C
    • Frozen samples, sub freezing outdoors
      • Shattered vials
      • Headspace when thawed
  • Contamination of Samples
    • Wash hands prior to sampling
    • Please make sure clothes and well house do not have VOCs
    • Test is very sensitive, if you have a weed-eater in the well house or recently filled with gas, you could contaminate the sample. DO NOT LET THIS HAPPEN TO YOU!

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How Much Headspace is too Much?

  • Large headspace
    • Lab will reject samples and send a new kit
  • Pea size
    • Lab will accept sample and qualify data (28 qualifier)

Pea size headspace:

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VOC Sample Collection to Help Prevent Headspace

  • Slowly fill vial to the point where you get a “domed meniscus”

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VOC Sample Collection to Help Prevent Headspace

  • What if a small amount of the sampled water runs over and down the side?
    • This is acceptable, it’s not enough to affect preservation

  • Chlorinated supply, have to use the clear vials first
    • What if I don’t get a “domed meniscus”?
    • Add additional sample into the clear vial to slowly top off the amber vial

  • Carefully replace and tighten the cap
    • Again, it may run down the sides of the container however, this is acceptable
    • Cap should be sufficiently tight to prevent air entrainment when sample is cooled

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Synthetic Organic Compounds (SOC)

  • Several Methods/Containers
    • 507/508
      • Single 1 L amber glass
    • 515.4
      • Two (2) – 40 mL amber glass
    • 531.1
      • Single 20 mL amber glass
    • Some have preservatives, do not rinse
  • Every 10 sample kits, randomly selected
    • Laboratory Quality Control
      • Field Blanks for each method, do not open these containers
      • Additional sampling in duplicate containers provided

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SOC Containers

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Common Issues with SOC Kits

  • Temperature
    • Samples must be received at, or below, 6°C
    • Large volume containers
    • Ice packs alone will not cool the samples to 6°C
    • Refrigerate samples overnight (or ice bath) prior to packing kit
    • Freeze ice packs overnight

  • Breakage
    • All containers for SOCs are glass
    • Each container is wrapped with padding
    • Shipping vendors sometimes abuse the kits
    • Broken containers must be resampled

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Disinfection Byproducts (DBPs)

  • Trihalomethanes (THMs)
    • Amber glass vials – two (2) - 40 mL
    • Each vial has granular preservative, sodium thiosulfate
    • Common issue is excessive headspace
      • Use same collection procedures discussed with VOC kits

  • Haloacetic Acids (HAAs)
    • Single 40 mL amber glass vial
    • Small volume of liquid preservative

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DBP Containers

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Lead and Copper Sampling

  • Samples collected in 1 L clear Nalgene containers
    • Samples taken in the distribution system of a residence or business
    • Strict monitoring period, samples must be collected between June 1 and September 30
    • Water systems are responsible for return shipping costs
      • No charge for shipping if you use the DHSS courier
    • Lab receives more than 6,000 bottles between June 1 and September 30
      • All kits are sent as a single, large shipment via UPS®, usually around May 30
      • Water systems should have the kits in early June

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Lead and Copper Sampling

    • Samples preserved at the laboratory with a six month holding time
      • No temperature requirements, samples are stored at room temperature
    • Logistical challenges for the lab
      • Storage and subsequent distribution of samples to the laboratory prior to analysis
      • Quantity of samples in a short period of time challenges instrument and personnel
      • Strive to turn around samples as quickly as possible
      • Samples received by the lab prior to August 1 have a quicker turnaround time

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Lead and Copper Average Turnaround Time

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Common Issues with Lead and Copper Samples

  • Receiving incomplete orders
    • Please wait to ship until all of your bottles have been returned
    • No need to place bottles in Ziploc® bags

  • Bottles are not completely full

  • Chain of Custody
    • Illegible handwriting
    • Tiers incomplete, not filled in

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Challenges with UPS Shipping

  • Sample breakage and cooler leakage
    • UPS will discard any package that is leaking liquid
  • Lost or diverted packages
  • Uncontrolled temperature in warehouses
    • Never send a kit with UPS on a Friday
    • Refrigerate samples and send on following Monday
  • Call tags
    • If UPS drivers do not stop to pick up kits, please let us know
    • Laboratory has changed its call tag procedures

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New Call Tag Procedures

  • Laboratory ships kits via UPS to water systems
    • Monday through Thursday only, all kits should arrive by Friday

  • Call tags are issued for the kits on Friday of that week
    • UPS will pick up the kits the following Monday, Tuesday or Wednesday
    • Contact us if UPS does not pick up the kit by Wednesday
      • Tonya Toebben – (573) 526-3327 or tonya.toebben@dnr.mo.gov
      • Sample Receiving – (573) 526-3333

  • New procedures avoid late week pickups
    • Samples will not sit in a hot or cold warehouse over a weekend

  • Please contact us with any questions on call tags

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DHSS Courier Service

  • DHSS has a courier network for transport of lab samples

  • Pros - Service is extremely reliable
    • Designated locations to drop off kits
    • Laboratory receives the kits the next morning
    • Samples stay in a temperature controlled environment
    • Glass container breakage is very rare
    • Most reliable and efficient way to return sample kits

  • Cons - Not as convenient as UPS call tags
    • Requires kits to be driven to drop off locations, with the nearest location many miles away

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Water Sampling Kits from the Lab Perspective

Questions?

Sampling kit contact information

Tonya Toebben Kevin Thoenen

Laboratory Support Supervisor Chemical Laboratory Manager

(573) 526-3327 (573) 526-6971

tonya.toebben@dnr.mo.gov kevin.thoenen@dnr.mo.gov