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  • Regulation 85

    NavigatingRegulation85PartIILabMethodsandDataSubmission

  • Presented By:Colorado Water Quality Monitoring Council (CWQMC)

    andColorado Monitoring Framework (CMF)

  • rk (CMF)

  • Presenters

    Phil Russell LEWWTP

    Sherry Scaggiari City of Aurora

    Linda Chynoweth City of Aurora

    Julie Stahli Metro Wastewater

  • What Are We Sampling?

    Phosphorus

    Nitrogen

    Flow

  • Effluent SamplingALL Dischargers

    Phosphorus: Total Phosphorus

    Nitrogen: Total Nitrogen (TN) andTotal Inorganic Nitrogen (TIN)

    Flow: Total daily flow (in gallons or MGD) on the day that nitrogen and phosphorus samples are collected. Typically the same value as in permit.

  • Stream SamplingDischargers > 1 MGD

    Phosphorus: Total Phosphorus

    Nitrogen: Total Nitrogen (TN)

    Flow: Daily average flow (cfs, typically from a downstream gaging station).

  • Total Nitrogen (TN) = TIN + TONOr

    Total Inorganic Nitrogen (TIN) = NH3 + NO3 + NO2

    Total Organic Nitrogen (TON) = TKN NH3

    So, TN = NO3 + NO2 + TKN

  • BottomLine

  • Detection Limits & Sample TypeUpstream & Downstream (mdl)

    Total Phosphorous 0.01 mg/LNitrate + Nitrite (N) 0.02 mg/LTKN 0.1 mg/LTN 0.1 mg/L

  • Effluent (PQL)

    Total Phosphorous 0.01 mg/LNitrate + Nitrite (N) 0.5 mg/LTKN 0.5 mg/LTN 0.5 mg/LNH3 0.05 mg/L

  • Regulation 85

    QUESTIONS?

  • MDLsandPQLsand

    ChoosingaLab

  • MDLMethodDetectionLimit

    40CFR136,AppendixB,definitionofMDL:

    Themethoddetectionlimit(MDL)isdefinedastheminimumconcentrationofasubstancethatcanbemeasuredandreportedwith99%confidencethattheanalyteconcentrationisgreaterthanzeroandisdeterminedfromanalysisofasampleinagivenmatrixcontainingtheanalyte.

  • What does that mean?

    A result greater than the MDL means the sample has a concentration greater than zero.

    NOT that the concentration is greater than the MDL.

    The method to calculate MDLs is specified in 40 CFR Part 136 Appendix B

    MDL is detection, not quantitation

  • Reg 85 MDLs

    Required MDLs are specified in Reg85 for all stream analytes

    (refer to previous section)

  • PQL

    Practical Quantitation Limit

    The lowest level that can be reliably achieved within specified limits of precision and accuracy during routine laboratory operating conditions

    EPA.gov NPDES Glossaryhttp://cfpub.epa.gov/npdes/glossary.cfm?program_id=0

  • PQL

    PQL is set by the state as the level that your

    chosen method must be able to

    meet.

    PQLs were listed in the previous section.

  • RL Reporting Limit

    The lowest quantified level within an analytical methods operational range deemed

    reliable enough, and therefore appropriate, for reporting by a laboratory

    Standard Methods 22nd Edition, 1010C

  • RL Reporting Limit

    ReportingLimitisQuantitation

    The level that we can quantitatively say the analyte

    exists at that concentration.

  • RLIt comes down to what concentration the laboratory feels comfortable saying they can quantify, confidently, on a daily basis.

    The final arbiter of the RL is the concentration of the lowest standard analyzed for that sample set.

    Laboratories almost universally have set their RL to the concentration of that lowest standard.

    Region III Quality Assurance MDL Fact Sheet http://www.epa.gov/region3/esc/qa/pdf/whatthel.pdf

  • PQL and RL

    If the PQL is set at 0.5mg/L:

    Case 1: the lab reports an RL = 0.5 mg/L that will work

    Case 2: the lab reports an RL at 0.4mg/L that will work, but you could ask them to report your data at 0.5 mg/L.

    Case 3: the lab reports an RL at 0.6 mg/L that method or lab MAY not work. You could consult with the lab and find out if it is possible for them to lower their RL. They have to set up a special method for you and run standards at the 0.5 mg/L level.

  • Reporting resultsPQL is 0.5 mg/L, MDL is 0.1 mg/L

    Case 1: result is 0.60 mg/L report 0.6 mg/L

    Case 2: result is 0.50 mg/L report 0.5 mg/L

    Case 3: result is 0.42mg/L report 0.4 mg/L, J

    Case 4: result is 0.09 mg/L report

  • Choosing a Lab or method

    Large list of methods (see SAP) Title40,Part136,Section136.3

    Laboratory Choice: Internal Abilities Many contract labs

  • Method Choice The method must be followed according to its

    reference (EPA, Standard Methods, etc) The method must be capable of meeting the MDL

    requirements. (40 CFR Part 136 Appendix B) All QC for the method must be followed. This is not

    bench or operational testing. Generally blanks, spikes (a sample made up with

    a known quantity) and duplicates are required. If a calibration curve is needed for the method, it

    must adhere to the requirements for number of standards and correlation coefficients.

  • InternalAbilities Assesswhetherornotyourpersonnelhavetheskills,time,spaceandequipmenttoanalyzetheseparameters.

    Comparecostswithacontractlab.

    MDL studiesmustbedoneinaccordancewithCFR

  • QuestionsfortheLab Which Method Numbers are run? What are their MDLs and PQLs? Are they using 40 CFR Part 136 Appendix B

    to determine their MDLs? If not, then how are they being calculated?

    While there is no official certification, labs should be doing blind performance testing (i.e. USGS Round Robin, DMRQA). Ask them for the most recent results for the

    parameters you are requesting.

  • Questions for the Lab

    What is the procedure for ordering bottles or sample kits? How much lead time is needed? Is there a preservative? Is the preservative added by the lab or the

    sampler? Do the samples need to remain at a given

    temperature? What is the sample holding time?

  • Questions for the Lab

    When is the best time to sample? If you have to ship samples can the lab

    accept on Saturdays?

    If you sample late in the day, can you still get samples to the lab? How late can they accept them?

  • Grabvs Composite

    GrabSamples:upstreamanddownstreamsamples couldalsobeeffluentsample.

    CompositeSamples:effluentsamplesareusuallygoingtobecompositesamples.

  • Grab Samples

    Typically one bottle for each parameter. Preservative

    If preservative is already in the bottle DO NOT RINSE

    If not, then rinse the bottle with sample three times before filling the bottle.

    Observe all requirements for chilling and transporting samples.

  • Composite samples

    Can be a mechanical compositor or timed grab samples.

    Can be used on Effluent Must collect sufficient

    volume for all tests. Evenly spaced samples

  • Composite Samples Ifusing grab samples, pour each grab into one main

    container or carboy.

    Keep good records of time, amount and flow

    Once all grab samples have been combined, mix the composite sample thoroughly and pour into bottles for required analyses.

    Preserve samples If pre-preserved bottles do not overflow

    If not preserved leave room for preservative.

    Observe all requirements for chilling and transporting samples.

  • Sample Preservation The stability of a sample depends on how

    well it is preserved. Proper preservation includes the use of the

    correct containers, pH control, protection from light, absence of head space, chemical addition, and temperature control.

    The chemistry of all analytes must be considered, recognizing that certain reactions may still occur under recommended preservation conditions.

  • Sample Preservation

    The objective is to provide the lab with a set of samples that closely represents the aquatic environment from which they were taken.

    To ensure consistency and efficiency, sample handling, preservation, storage, and transportation procedures must be followed and documented.

  • Holding Time

    Holding time is the length of time a sample can be stored after collection and preservation, and before preparation and analysis, without significantly affecting the analytical results.

    Holding times vary with the analyte, preservation technique, and analytical method.

  • Fieldduplicatesandfieldblanks

    oneeachforevery20samples(10%ofsamples)collected

    thefieldduplicateiscollectedimmediatelyaftertheprimarysampleiscollectedatthesite.

    Fieldblanksaretakenbypouringreagentwaterfromthelaboratoryintosamplebottlesatthesite.

    Reagentwaterwouldneedtoberequestedfromthelaboratory.

    Fieldduplicates/blanksarelabeledasseparatesamplestoavoidconfusionandtoprovideanunbiasedblindevaluation.

    RecommendedFieldQA/QC

  • The ability to trace possession and handling of the sample from the time of collection to laboratory

    testing and then to final disposition.

    Chain of Custody

  • Regulation 85

    QUESTIONS?

  • DataSubmission

  • Minimum Data Elements

    Typically a minimum set of elements for your data in four categories: Organization information Information on your monitoring project Monitoring locations Results

  • Data Template

    An excel spreadsheet can be used for the minimum data elements. The tabs on your excel spreadsheet will be the four categories.

    Example:

    CharacteristicName MethodSpeciationResultSample

    FractionResultValue ResultUnit

    AmmonianitrogenasN

    Total mg/l

    Nitrate asN Total 7.2 mg/l

    Nitrite asN Total 5.46 mg/l

    Kjeldahlnitrogen asN Total 12.3 mg/l