qualifiers hplc/ic metals rad
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From: Mahler, TomTo: StGermain, MargieCc: Velasquez, Isabel; Fries, Harvey; Adkins, TabathaSubject: RE: Final details of SwRI"s verification analyses of Test America dataDate: Monday, April 17, 2017 10:20:00 AM
Margie,I am providing the information related to qualifiers in the laboratory data that ENST is currentlysupporting SUPR with a review.Below are the qualifiers as defined by Test America:QualifiersHPLC/ICQualifier Qualifier DescriptionF1 MS and/or MSD Recovery is outside acceptance limits.J Result is less than the RL but greater than or equal to the MDL and the concentration is an approximate value.E Result exceeded calibration range.MetalsQualifier Qualifier DescriptionB Compound was found in the blank and sample.J Result is less than the RL but greater than or equal to the MDL and the concentration is an approximate value.F1 MS and/or MSD Recovery is outside acceptance limits.F2 MS/MSD RPD exceeds control limits4 MS, MSD: The analyte present in the original sample is greater than 4 times the matrix spike concentration; therefore,control limits are not applicable.RadQualifier Qualifier DescriptionU Result is less than the sample detection limit.X Carrier is outside acceptance limits.G The Sample MDC is greater than the requested RL.X Tracer is outside acceptance limits.Rad TICsQualifier Qualifier DescriptionU Result is less than the sample detection limit.Below are the qualifiers for the SwRI data:Data Reporting Qualifiers (Qual)J - Result is greater than or equal to the Limit of Detection (LOD) and less than the Limit of Quantitation (LOQ)U - Result is less than the SwRI Reporting Limit (RL)N - Matrix spike and/or matrix spike duplicate criteria was not metX - Analytical spike criteria was not metE - Result is estimated due to interferencesD - Result is reported from a dilution* - Duplicate criteria was not metJ- and J+ qualifiers are likely applied by the PRPs and take no additional meaning other than what isdefined above except the “-“ indicates they believe the estimate is biased low and the “+” indicatesthe estimate is biased high.Let me know if there are any other questions,Tom
From: StGermain, Margie Sent: Tuesday, April 11, 2017 2:38 PMTo: Mahler, Tom Cc: Velasquez, Isabel ; Fries, Harvey ; Adkins, Tabatha Subject: FW: Final details of SwRI's verification analyses of Test America dataDo you have a list of the qualifier codes used in the spreadsheet in column I? The codes include: N, J,J-, D, and U.Please reply all so the chemists receive the answer directly.
Margie St. GermainLaboratory DirectorSTC/ENST/LTAB913-551-5154From: Fries, Harvey Sent: Tuesday, April 11, 2017 12:46 PMTo: StGermain, Margie ; Velasquez, Isabel Cc: Adkins, Tabatha Subject: RE: Final details of SwRI's verification analyses of Test America dataMargie,Do you have a list of the result qualifier codes used in the spreadsheet?Regards,Harvey
From: StGermain, Margie Sent: Thursday, April 06, 2017 4:06 PMTo: Velasquez, Isabel <[email protected]>; Fries, Harvey <[email protected]>Cc: Adkins, Tabatha <[email protected]>Subject: FW: Final details of SwRI's verification analyses of Test America dataMargie St. GermainLaboratory DirectorSTC/ENST/LTAB913-551-5154From: Mahler, Tom Sent: Thursday, April 06, 2017 2:08 PMTo: StGermain, Margie <[email protected]>Subject: FW: Final details of SwRI's verification analyses of Test America dataSee the email below regarding the summary of Superfund’s direction to SwRI in regards to thesample analyses.As I mentioned in my previous email, I believe this information will be useful for the data reviewers.Let me know if there are any more questions,Tom MahlerOn-Scene CoordinatorUS EPA Region 7913-551-7416
From: Mahler, Tom Sent: Friday, August 05, 2016 4:33 PMTo: [email protected]: Juett, Lynn <[email protected]>; Vann, Bradley <[email protected]>; Stoy, Alyse<[email protected]>; Rob Monnig <[email protected]>Subject: Final details of SwRI's verification analyses of Test America dataPaul,As we have discussed previously, I am providing further details as to the specific analyses that EPAintends to have Southwest Research Institute (SwRI) perform on the samples collected in Januarythat were sent to Test America. For clarity, I am referring specifically to the remaining samplematerials associated with Test America lab reports #160-15607-1 and #160-15609-1 that wereprovided to SwRI.
As I have previously stated in my July 15, 2016 email, EPA’s intent is for these samples to be analyzedin a manner consistent with the procedures that Test America followed as documented in thepreviously mentioned lab reports in order to verify certain results. Careful consideration of thedocumentation associated with these samples, the current capabilities and practices of SwRI, as wellas additional input from EPA scientists have been combined in order to create a list of analyses thatEPA feels is appropriate to verify Test America’s results. I have provided this list below as well as anexplanation for each analysis.
1. Isotopic Thorium by DOE A-01-R (alpha spectrometry) – This will include results for Th-232, Th-230, and Th-228. It will be conducted consistent with Test America’s methodology.
2. Isotopic Uranium by ICP-MS – This will include results for U-238, U-235, U-234, and Th-230.This analysis will be conducted consistent with the methodology SwRI performed on EPA’ssamples utilized for the radon emanation portion of the pyrolysis study. This data and theassociated documentation is available on EPA’s West Lake Landfill web page. This is alsoconsistent with what I have communicated to you in my July 15, 2016 email. SwRI has indicatedthat they can also provide a result for Th-230 that will not require any additional samplematerial. They have indicated that this can be achieved with appropriate calibration of equipmentand laboratory standards. All the documentation associated with this analysis will provided to youconsistent with level 4 data reporting.
3. Radium by EPA Method 901.1 (gamma spectroscopy) – This will include results for Ra-228and Ra-226 via in-growth of their decay progeny. This will also include a variety of other gammaemitting radionuclides consistent Test America’s analysis. At this time, EPA is not requestingSwRI to perform either method 903.0 (GFPC) for Ra-226 or method 904.0 (GFPC) for Ra-228.This is because of potential interferences that occur during the extraction step related to thepresence of elevated Barium in the samples which have been identified by Test America andSwRI. EPA also notes that the minimum detectable concentrations that can be achieved viagamma spectroscopy are adequate to characterize the amount of Ra-226 and Ra-228 in thesesamples. Furthermore, this is a non-destructive technique. I am happy to discuss this in moredetail if there are additional questions.
4. Pb-210 by Gas Flow Proportional Counter (GFPC) – EPA is requesting that SwRI performPb-210 analysis by GFPC instead of ST-RC-0211 (Liquid Scintillation Counter or LSC). This isbecause SwRI routinely analyzes soil samples for Pb-210 via GFPC. SwRI expects that thisanalysis will yield a lower detection limit with fewer interferences and less error than LSC. In aneffort to minimize delays, EPA feels this method is acceptable and will yield comparable results.
5. Mercury by EPA Method 7571B – No change from the Test America method6. Fluoride/Sulfate by EPA Method 9056 – No change from the Test America method7. pH by EPA Method 9045D – No Change from the Test America method8. Alkalinity by MOSA 2nd Edition, Chapter 10-3.2 – Because EPA Method 310.1 is applicable to
drinking, surface, and saline waters, domestic and industrial wastes, it does not prescribe theextraction necessary to apply this method to a soil sample. Because the details of the extractionstep are known to EPA at this time, SwRI is recommending that this analysis be performed viaMOSA (Methods of Soil Analysis). Again, documentation of this analysis will be providedconsistent with level 4 data reporting.
9. Metals including scandium, niobium, and tantalum by EPA Methods 6010B and 6020with digestion by EPA Method 3050B – SwRI will report scandium via method 6020 becausescandium is their internal standard for method 6010B.
10. Metals including scandium, niobium, and tantalum by EPA Methods 6010B and 6020with total digestion – Three sample digestion techniques will be utilized. One technique is aclosed vessel digestion using concentrated nitric, hydrochloric and hydrofluoric acids. Anothertechnique is a lithium metaborate/tetraborate fusion. The third technique is performed usingconcentrated nitric, perchloric, hydrofluoric and hydrochloric acids in an open vessel. This testwill require a small amount of sample material but EPA believes there will be plenty of samplematerial to perform this test given that we intend to test for radium via a non-destructivemethod. Digestion by EPA Method 3050B is “not a total digestion technique for most samples.It is a very strong acid digestion that will dissolve almost all elements that could become‘environmentally available’.” (See page 1 of EPA’s 3050B document,https://www.epa.gov/sites/production/files/2015-06/documents/epa-3050b.pdf) Due to the
nature of this material, this method will provide a second set of metals results, in particularfor barium, that may be useful to better understand potential discrepancies between SwRIand Test America’s results.
EPA intends to direct SwRI to perform these analysis by the end of next week. Please let me know ifthere are any questions or concerns.Tom MahlerOn-Scene CoordinatorUS EPA Region 7913-551-7416