UNITED STATES ENVIRONMENTAL PROTECTION AGENCY REGION III 841 Chestnut Bundling Philadelphia, Pennsylvania 19107 SUBJECT: Region 3 Superfund Data Validation DATE: MUU • 6 ^95 Policy1 - FROM: Abe Ferdas, Associate Director /^b<£~'\^' Office of Superfund Programs (3HW02) TO: Superfund Program Staff Purpose: The Environmental Protection Agency makes consequential decisions regarding public health and environmental conditions. Analytical data are the cornerstone of this Agency's decision making processes. Thus, it is imperative that the data used in these processes be of known and documented quality. The quality of analytical data is determined through the data validation process. Specifically, data validation is a systematic procedure for reviewing analytical data against a set of established criteria to determine its validity relative to the data's intended use. The purpose of this memo is to clearly define this Region's data validation policy for the Superfund program. Background: Each environmental data collection activity is different due to elements of variability which include site history, project objectives, and the amount of historical data available. The. Site-specific procedures for data validation are specified in the individual Sampling and Analysis Plans developed for each site. Organizations performing environmental data collection activities should specify data validation requirements. These requirements should adequately support the intended use of the data. 1 This policy and the procedures set out in this document are intended for the use of U.S. EPA response personnel. EPA reserves the right to change this Policy at any time, without prior notice, or to act at variance with this policy. This policy does not create any rights, duties or obligations, implied or otherwise, in any third parties. ------- Implementation: Data review/validation procedures for this Region are delineate'd in: • Region III Modifications to the National Functional Guidelines for Organic Data Review • Region III Modifications to the Laboratory Data Validation Functional Guidelines for Evaluating Inorganic Analyses. These procedures provide the reader with instructions on how to perform a full data validation. EPA Region III advocates full data review/data validation to support quantitative Superfund Baseline Risk Assessments. This data validation is performed by an independent party other than the laboratory that generates the analytical data. The validation is performed on all (100%) of the data. The appropriate qualifiers should be applied to 100% of the data. There are various EPA national guidance documents that address the objectives for data review/validation. Risk Assessment Guidance for Superfund. Volume 1 and the Guidance for Data Useability in Risk Assessment include discussions of data quality as a function of data use. For quantitative risk assessment, EPA National Guidelines indicate a preference for full data review. For uses of data other than quantitative baseline risk assessment, the degree or intensity of data validation may vary based upon the intended use of the data. Region Ill's "Innovative Approaches to Data Validation" supports this concept. The Region's primary goal is to verify that the data quality produced is adequate for the intended data use. The "Innovative Approaches to Data Validation" defines levels of data review which are based on how data are to be used. Each review level contains data validation evaluation criteria which support the data use category. However, it is important to note that under all circumstances the following conditions should be met: • The analytical deliverable requirement must contain all of the documentation listed in Appendix A of this memorandum. • Data qualifiers are applied to 100% of the data in all cases. • All data used to support quantitative baseline risk assessment should be reviewed using full Region III data validation procedures. The Region encourages dialogue between EPA and PRPs during the scoping phase of a project to establish site-specific data ------- quality objectives that will meet the needs of each data collection activity. It should be emphasized that the scoping phase of the remedial process is the best time to present and discuss the data validation objectives of the project. An early and comprehensive discussion of the data validation procedures of the project will reduce the uncertainty during risk assessment. The final decision regarding the appropriate level of review must be approved by the EPA project manager. Summary: • Site specific data validation objectives are specified in the sampling and analysis plan for each site. • Region III advocates 100% data validation to support any quantitative baseline risk assessment developed for the Superfund program. • For data uses other than quantitative baseline risk assessment, Region III Innovative Approaches may be used with EPA project manager approval. • Data validation procedures are provided in the Regional Guidelines as noted above. ------- Appendix A ------- The contents of a data validation package are as follows: Narrative The narrative describes and summarizes the results of the analytical process. It is composed of: Overview - Describes the sample set (e.g. number of samples, matrices) and informs the user of the method of analysis. summary - Provide* a synopsis of the sample analysis and advises the user of any unsuccessful analyses. Xajor issues - Presents issues which directly affect data quality in an adverse manner. Kay include statements regarding suspect and unusable data, or problems concerning sample integrity. Minor issues - Summarizes data qualifiers that have been applied to positive values or quantitation limits and informs tae user of the limitations of data use. Attachments Each report must have the following attachments: Appendix A - Glossary of data qualifiers Appendix B - Data Summary Forms (Regional data summary forms are available from the Quality Assurance Branch.) Appendix C - Results as reported by the laboratory (Form 1 or equivalent) Appendix D - Results of all Tentatively Identified Compounds which have been corrected to exclude blank contamination (Organics only) Appendix E - Support documentation which substantiates qualifiers placed on data during review (i.e. method blanX forms/ calibration forms, quantisation reports). ------- Deliverables Listing Metals Analyses I. Chain of Custody II. Narrative - Describe analyses performed and discuss any problems associated with the data reported. III. Sample Results (for each sample) sample number date received matrix % solids (for non-aqueous samples only) concentration units metal and determined concentration IV. QC Data (for those QC samples required by the method used to determine the metals analyzed for) .' 0 Initial and Continuing Calibration Results source of calibration standard(s) concentration units true value (for each analyte) measured value (for each analyte) percent recovery (for each analyte) 0 CRDL Standard Recoveries for AA and ICP. (These analyses are required under the CLP protocols, other methods may or may not require that a standard at or near the detection limit of the instrument be analyzed to verify acceptable performance at that concentration level. If the method does not require such an analysis than this form is omitted.) same as listed for initial and continuing calibration 0 Blanks preparation blank matrix instrument and preparation blank units initial calibration blank results continuing calibration blank results preparation blank results ------- ICP Interference Check Sample (only needed if any analytes are determined by ICP methods) ICP instrument ID (only if more than one ICP) concentration units true values (for each analyte and solution) found values (for each analyte and solution) percent recovery (for each analyte) Matrix Spike Sample Recovery matrix concentration units control limit ^ spike sample result 'unspiked sample result amount of spike added percent recovery Post Digest Spike Sample Recovery. (These analyses are required under the CLP protocols, other methods may or may not require that a post digest spike sample analysis be performed when the pre-digestion spike recovery is outside acceptable limits. If the method does not require such an analysis than this form is omitted) same as for matrix spike recovery Duplicates (note: for laboratory duplicate analysis results only) matrix percent solids for sample and duplicate (if non-aqueous matrix) concentration units control limit sample results duplicate results relative percent difference (% RPD) Laboratory Control Sample matrix concentration units true value found value percent recovery control limits (if applicable) ------- 0 Method of Standard Addition Results (for each analyte result determined by MSA) sample no. analyte 0 ADD ABS 1 ADD and ABS 2 ADD and ABS 3 ADD and ABS final cone. correlation coefficient 0 ICP Serial Dilutions (only if ICP methods were used) matrix concentration units initial sample result serial dilution result (corrected for dilution) percent difference 0 Instrument Detection Limits instrument ID's wavelength type of background correction instrument detection limit 0 ICP Interelement Correction Factors (only if ICP methods were used) wavelength correction factor by analyte/interfering analyte 0 ICP Linear Ranges (only if ICP methods were used) V. Raw Data For each reported value, the laboratory should include in the data package all raw data from the instrument used to obtain the sample values and the QA/QC values reported (except for raw data for quarterly verifications of instrument parameters such as IDLs and interelement correction factors). Raw data must contain all instrument readouts used for the sample results, including those readouts that may fall below the IDL. All AA and ICP instruments should provide a legible hard copy of the direct real-time instrument readout (i.e., stripcharts, printer tapes, etc.). A photocopy of the ------- direct sequential instrument readout must be included. A hardcopy of the direct instrument readout for cyanide should be included if the instrumentation has the capability. All raw data should include intensities (ICP) and absorbances (AA) with concentration units (unless instrument direct readout is in concentration units). All flame and furnace AA data should be grouped by element. To facilitate data validation, it is recommended that the raw data be identified to identify the following: 0 Calibration standards, including source and prep date. 0 Initial and continuing calibration blanks and preparation blanks. 0 Initial and continuing calibration verification standards, interference check samples, and ICP serial dilution samples. 0 Diluted and undiluted samples (by sample number) and all weights, dilutions and volumes used to obtain the reported values. (If the volumes, weights and dilutions are consistent for all samples in a given data package, a general statement outlining these parameters is sufficient). 0 Duplicates. 0 Spikes (indicating standard solutions used, final spike concentrations, volumes involved). If spike information (source, concentration, volume) is consistent for a given data package, a general statement outlining these parameters is sufficient). 0 Instrument used, any instrument adjustments, data corrections or other apparent anomalies on the measurement record, including all data voided or data not used to obtain reported values and a brief written explanation. 0 All information including date for furnace analysis clearly and sequentially identified on the raw data, including sample number, sample and analytical spike data, percent recovery, coefficient of variation, full MSA data, MSA correlation coefficient, slope and y intercept of linear fit, final sample concentration (standard addition concentration), and type of background correction used. ------- 0 Time and date of each analysis. Instrument run logs can be submitted if they contain this information. If the instrument does not automatically provide times of analysis, these should be manually entered on all raw data for initial and continuing calibration verification and blanks, as well as interference check samples and linear range analysis. 0 Integration times for AA analyses. VI. Digestion and Distillation Logs Digestion and distillation logs for all samples analyzed should be submitted. These logs should include: (1) date, (2) sample weights and volumes, (3) sufficient information to unequivocally identify which QC samples^i.e., laboratory control sample, preparation blank) correspond to each batch digested, (4) comments describing any significant sample changes or reactions which occur during preparation, and (5) indication of pH <2 or >12, as applicable. ------- Deliverables Listing Organic Analyses .1. Chain of Custody II. Narrative - Describe analyses performed and discuss any problems associated with the data reported. III. Volatiles/Semi-Volatiles Data QC Summary - Surrogate Recovery Summary - Matrix Spike/Matrix Spike Duplicate Recovery Summary - Method Blank Summary (list associated samples for each method blank) - Tuning Summary for BFB and DFTPP . in chronological order by instrument Sample Data (for each sample) - Form I (from Org. SOW) or Lab Generated Reports header must include the following: sample no. date received matrix units.reported amount of sample date extracted (Semi-VOA only) % Moisture (soils only) pH (waters only) . - Reconstructed Ion Chromatogram (RIC) label internal and surrogate standards normalize to highest non-solvent peak header must include to following: sample no. date and time of injection instrument ID lab file ID - Quantitation Reports header must include: same as for RIC dilution factors amount injected - Compound Identification (for all compds. detected except surrogates and internal standards) - Raw mass spectra • - background subtracted mass spectra1 - standard spectra , • ------- Standards - Initial Calibration Form include: date calibrated time calibrated applicable file IDs response factors for each compound at each level mean response factor Percent Relative Standard Deviation (%RSD) - RIC/Chromatogram and Quantitation report for each standard in initial calibration in chronological order by instrument - Continuing Calibration Form include: date and time calibrated mean response factor from initial calib. response factor from continuing calib. percent difference (%D) *- Internal Standard Area Summary in order by instrument include: continuing calib. internal standard areas cont. calib. internal std. retention times internal standard areas and retention times for all samples quantitated against continuing calib, Raw QC - Tuning BFB/DFTPP ... bar graph spectrum mass listing - Blank Data - Form I or lab generated report forms for each method blank - RIC/Chromatogram - Quantitation report - Mass Spectrum of each positive result (above same header as samples) - Matrix Spike/Matrix Spike Duplicate Data - Form I or lab generated report forms - RIC/Chromatogram - Quantitation report - spectra not required Copies of Sample Preparation/Extraction Logbooks Run log/Injection logbook 11 ------- IV. Pesticide/PCB Data QC Summary - Surrogate Recovery Summary - Method Blank Summary - Matrix Spike/Matrix Spike Duplicate Recovery Summary Sample Data - Form I or lab generated report forms - Chromatogram header must include: sample no. volume injected date and time of analysis column instrument identification all positives labelled - Confirmation Chromatogram (if applicable) header same as above - GC integration report - GPC Chromatogram (if performed) - GC/MS Spectra (if confirmation on GC/MS performed) Standards Data - Pesticide Evaluation Standards Summary - Pesticide/PCB Standard Summary include: calibration factors percent difference (%D) for continuing and initial calib. , - Pest/PCB standards data - Chromatogram and integration reports in chronological order by instrument label all peaks for individual compounds list total ng injected retention time and peak areas date and time injected GC column ID GC instrument ID ii-i ------- Raw Data Blank Data - Form I or lab generated result form - chromatogram - integration reports in chronological order Matrix Spike/Matrix Spike Duplicate - Form I or lab generated result form - chromatogram - integration reports IV ------- |