Pete the penguin says

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Pete the penguin says

• Before the show begins, dont forget to visit
  the snack bar

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(No Transcript)
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MDEQ DRO/ORO Analysis

• 8015 GC/FID

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EPA 8015 and Wisconsin 8015

• These methods define Diesel Range Organics, DRO,
  as anything eluting between C10 and C28
• No other carbon ranges included

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An example chromatogram of diesel fuel using
C10-C28
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Why change?

• This chromatogram looks OK, doesnt it?

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2000 ppm 10W30 Oil old method

• Much of this material is included in the C10-C28
  range

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Why change?

• Maybe this chromatogram doesnt look so good, a
  lot of oil is being defined as Diesel Range
  Organics.

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Why change? (What are the current problems?)

• Theres still space left on the run
• The diesel is gone before C28
• The motor oil is half included in the diesel
  range

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Why change? (What are some solutions?)

• Define DRO as C10-C20
• Add Oil Range Organics as C20-C34

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1000 ppm Diesel Fuel new method

• Most of the diesel (gt90) is contained within the
  range

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2000 ppm 10W30 Oil new method

• Much of this material would be included in the
  C10-C28 range, but now has a place of its own

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Why change? (What are some outcomes)

• Better description of contaminant
• There are no regulatory criteria, so its all
  about aesthetics

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Technical Details Overview

• This analysis has some specific differences from
  normal chromatographic analyses
• Have an open mind
• The quantitative results are going to be used for
  guidance, not necessarily for regulatory
  compliance

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Technical Details Integration/Calibration

• Baseline is drawn horizontally
• All material under the signal is included
• Do not integrate valley to valley
• 8015 allows for baseline subtraction to account
  for column bleed but
• Calibration by linear regression accounts for
  bleed without need for subtraction

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Technical Details Surrogate n-Eicosane (C20)

• Why C20?
• C20 is the dividing point between the two analyte
  fractions
• C20 is in a good range to determine accurate
  extraction recovery
• Easier to use area summing feature on software
  (pragmatic, not lazy)

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Technical Details Surrogate n-Eicosane (C20)
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Technical Details Surrogate Recovery

• Surrogate recoveries for high concentration
  samples, or samples containing unknown or
  degraded hydrocarbons should be considered
  estimated.

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Technical Details Surrogate Recovery

• A known amount of surrogate, n-eicosane, is added
  by the laboratory before extraction. N-Eicosane
  is also present in many petroleum products. If
  the product is a known material, the presence and
  quantity of n-eicosane can be accounted for. Our
  method includes calculations to make corrections
  for surrogate recovery based on concentrations of
  diesel fuel and motor oil in samples. In samples
  containing unknown or degraded materials the
  concentration on n-eicosane cannot be accounted
  for, therefore the calculation of surrogate
  recovery is and estimate.

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Technical Details Surrogate Recovery

• A known amount of surrogate, n-eicosane, is added
  by the laboratory before extraction.

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Technical Details Surrogate Recovery

• N-Eicosane is also present in many petroleum
  products.
• If the product is a known material, the presence
  and quantity of n-eicosane can be accounted for.
• Diesel fuel in our method has a 1.0 contribution
  from C20.
• 10W30 Motor Oil has a 0.22 contribution from
  C20.
• Our method has calculations to make corrections
  for surrogate recovery based on concentrations of
  diesel fuel and motor oil in samples.

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Technical Details Surrogate Recovery

• In samples containing unknown or degraded
  materials the concentration on n-eicosane cannot
  be accounted for, therefore the calculation of
  surrogate recovery is and estimate.

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Technical Details Surrogate Recovery

• A known amount of surrogate, n-eicosane, is added
  by the laboratory before extraction. N-Eicosane
  is also present in many petroleum products. If
  the product is a known material, the presence and
  quantity of n-eicosane can be accounted for. Our
  method includes calculations to make corrections
  for surrogate recovery based on concentrations of
  diesel fuel and motor oil in samples. In samples
  containing unknown or degraded materials the
  concentration on n-eicosane cannot be accounted
  for, therefore the calculation of surrogate
  recovery is and estimate.

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Technical Details Surrogate Recovery

• If the surrogate recovery is so estimated, why
  bother to use it?

• Surrogate works OK if sample contains diesel or
  10W30 and even better as the analyte levels
  decrease. If you have no analyte, the surrogate
  will give you a good measure of extraction
  recovery.

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Technical Details FID vs MSD

• Why cant we use GC/MS?

• You can! Just make sure to scan to a high enough
  mass to get signal from all the high molecular
  weight compounds.

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Technical Details Disclaimer

• This method defines only the carbon range of
  analytes. For example, a positive result for DRO
  does not indicate diesel fuel, only the presence
  of hydrocarbons in a boiling point range similar
  to, or encompassed by, diesel fuel.

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Ask a question
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2000 ppm 5W30 Oil new method
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2000 ppm 20W50 Oil new method