Appendix C Validation Standard Operating Procedures

1 Appendix C Validation Standard Operating Procedures Validation SOP Semivolatile Organics USEPA Region 2 SOP HW-35 Rev. 1 ~Ge~ChemiStHazousWasteSupportSectionDate '~7 Date:Date:Date:BranchWasteConcurredbY:~t =~PeerReviewedbY:~~~~~~~~~__Russe1 Arnone,ChemistHazaousWasteSupportApprove dby:I-----AnnualReviewReviewedby:NameDat e:Reviewedby: Semivolatiles SOP HW-35 EPA/Region IITABLE OF and COMPLETENESS AND Chain of Custody and Sampling Trip Data Completeness and Cover Letter SDG Data Validation A: VOA Sample Holding Deuterated Monitoring Compound (DMC) Recovery (Form II)64. Matrix Spike/Matrix Spike Duplicate Recovery (Form III)115.

2 Method Blanks (Form IV)..126. GC/MS Instrument Performance Check (Form V)..158. Target Compound List (TCL) Analytes (Form I)..189. Tentatively Identified Compounds (TIC)..2010. Compound Quantitation and Reported Detection Limits2111. standards Data (GC/MS)..2112 GC/MS Initial Calibration (Form VI)..2113. GC/MS Continuing Calibration Verification (CCV) (FormVII)..2414. Internal Standard (Form VIII)..2615. Field and ApplicabilityThis SOP offers detailed guidance in evaluating laboratorydata generated according to the method in the "USEPA ContractLaboratory Program Statement of Work for Organics Analysis Multi-Media, Multi-Concentration, , May 2005". The validationprocedures and actions discussed in this document are based onthe requirements set forth in the "USEPA Contract LaboratoryProgram National Functional Guidelines for Superfund OrganicMethods Data Review, January 2005".

3 This document attempts tocover technical problems specific to low/Medium concentration ofsemivolatile compounds. Situations may arise where datalimitations must be assessed based on the reviewer's ownprofessional judgement. In addition to technical requirements, contractual requirementsmay also be covered in this document. While it is important thatinstances of contract non-compliance be addressed in the DataAssessment, the technical criteria are always used to qualify theanalytical ensure a thorough evaluation of each result in a datacase, the reviewer must complete the checklist within this SOP,answering specific questions while performing the prescribed"ACTIONS" in each section.

4 Qualifiers (or flags) are applied toquestionable or unusable results as instructed. The dataqualifiers discussed in this document are as follows:Data QualifiersU - The analyte was analyzed for, but was not detectedabove the reported sample quantitation - The analyte was positively identified; the associatednumerical value is the approximate concentration of theanalyte in the - The analysis indicates the presence of an analyte forwhich there is presumptive evidence to make a"tentative identification."JN - The analysis indicates the presence of an analyte thathas been "tentatively identified" and the associatednumerical value represents its approximateconcentration.

5 12UJ - The analyte was not detected above the reported samplequantitation limit. However, the reported quantitationlimit is approximate and may or may not represent theactual limit of quantitation necessary to accuratelyand precisely measure the analyte in the - The sample results are rejected due to seriousdeficiencies in the ability to analyze the sample andmeet quality control criteria. The presence or absenceof the analyte cannot be Qualifiers:D - The positive value is the result of an analysis at asecondary dilution - The analyte is present in the associated method blankas well as in the sample. This qualifier has adifferent meaning when validating inorganic - The concentration of this analyte exceeds thecalibration range of the - Pesticide/Aroclor target analytes when the % Differencebetween the analyte concentrations obtained from thetwo dissimilar GC columns is greater than 25%.

6 The reviewer must prepare a detailed data assessment to besubmitted along with the completed SOP checklist. The DataAssessment must list all data qualifications, reasons forqualifications, instances of missing data and contract non-compliance. Reviewer Qualifications:Data reviewers must possess a working knowledge of the USEPAS tatement of Work and National Functional Guidelinesmentioned Operating Region II Date: August 2007 Method: CLP/SOW, SOP HW-35/SVOA, Revision 1S)))))))))))))))))))))))))))))))))))))) )))))))))))))))))))))))))))))))))))) ..YESNON/A3 PACKAGE COMPLETENESS AND DELIVERABLESCASE NUMBER: LAB: SITE NAME: SDG No(s).

7 : Chain of Custody and Sampling Trip Are the Traffic Reports/Chain-of-Custody Recordspresent for all samples?[ ] ACTION: If no, contact RSCC, or the TOPO to obtain replacement of missing or illegible copiesfrom the Is the Sampling Trip Report present for allsamples? [ ] ACTION: If no, contact either RSCC or ask the TOPO toobtain the necessary information from the Data Completeness and Have any missing deliverables been received and added to the data package? [ ] ACTION: Contact the TOPO to obtain an explanation orresubmittal of any missing deliverables from the lab.

8 If lab cannot provide them, note the effect on thereview of the data package in the ContractProblems/Non-compliance section of the Was CLASS CCS checklist included with thepackage? [ ] Standard Operating Region II Date: August 2007 Method: CLP/SOW, SOP HW-35/SVOA, Revision 1S)))))))))))))))))))))))))))))))))))))) )))))))))))))))))))))))))))))))))))) .. Are there any discrepancies between the TrafficReports/Chain-of-Custody Records, Sampling TripReport and Sample Tags? [ ] ACTION: If yes, contact the TOPO to obtain an explanation orresubmittal of any missing deliverables from Cover Letter SDG Is the SDG Narrative or Cover Letter Present?

9 [ ] Are case number, SDG number and contract numbercontained in the SDG Narrative or cover letter(see SOW, Exhibit B, section )?EPA sample numbers in the SDG, detaileddocumentation of any quality control, sample,shipment, and/or analytical problems encounteredin processing the samples? Corrective actiontaken? [ ] Does the Narrative contain the followinginformation , page B-12, section )?column used, storage of samples, case#, SDG#,analytical problems, and discrepancies betweenfield and lab weights. [ ] Did the contractor record the temperature of thecooler on the Form DC-1, Item 9 - CoolerTemperature, and in the SDG Narrative?

10 [ ] Does the Case Narrative contain the "verbatim" statement (page B-12, section of the SOM)?ACTION: If "No", to any question in this section, contact the TOPO to obtain necessary resubmittals. If unavailable, document under the Contract Problems/ Non-Compliance section of the Data Assessment.[ ] Standard Operating Region II Date: August 2007 Method: CLP/SOW, SOP HW-35/SVOA, Revision 1S)))))))))))))))))))))))))))))))))))))) )))))))))))))))))))))))))))))))))))) .. Data Validation Check the package for the following (see SOM reportingrequirements, section , page B-10): a.