SIXTH SAMPLING REPORT MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS August 1992 Prepared for Tutu Environmental Investigation Committee San Juan, Puerto Rico Prepared by Geraghty & Miller, Inc. 201 West Passaic Street Rochelle Park, New Jersey 07662 (201) 909-0700 GERAGHTY & MILLER. INC TUT °°3 *64434* 64434 SIXTH SAMPLING REPORT MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS August 27, 1992 Geraghty & Miller, Inc. is submitting this report to the Tutu Environmental Investigation Committee for work performed at the Tutu Wells Site in St. Thomas, U.S. Virgin Islands. The report was prepared in conformance with Geraghty & Miller's strict quality assurance/quality control procedures to ensure that the report meets the highest standards in terms of the methods used and the information presented. If you have any questions or comments concerning this report, please contact one of the individuals listed below. Respectfully submitted, GERAGHTY & MILLER, INC. Uma Parasar Scientist //fe*v-o-^f Thomas V. Danahy Senior Scientist/Project Manager Daniel A. Nachman Vice President/Project Officer TUT GERAGHTY & MILLER. INC. CONTENTS Page INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 SAMPLING AND ANALYTICAL PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . 2 TECHNICAL METHODOLOGY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 PROCEDURAL DEVIATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 DATA VALIDATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 ORGANIC ANALYTICAL RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 RECOMMENDATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 TABLES 1. List of Sample Locations and Analytical Parameters for the Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 2. Summary of Detected Volatile Organic Compounds in Ground-Water Samples Collected in May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 3. Concentrations of Volatile Organic Compounds in Ground-Water Samples Collected in May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 4. Volatile Organic Analysis Holding Time Summary, Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 5. Summary of Volatile Organic Compound Contaminated Blanks and Associated Ground- Water Samples, Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 6. Concentrations of Volatile Organic Compounds in Ground-Water Samples Collected from September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. GERAGHTY & MILLER. INC TABLES (Continued) 7. Summary of Detected Volatile Organic Compounds in Ground-Water Samples Collected from September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 8. Comparison of Applicable or Relevant and Appropriate Requirements with Detected Analytes in Ground-Water Samples Collected in May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 9. USEPA Maximum Contaminant Level Standards for Volatile Organic Compounds in Drinking Water. 10. Calculated Values for Relative Percent of PCE for Selected Supply Well Samples from September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 11. Proposed Sampling Locations and Analytical Parameters for the Seventh Sampling Event, September 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. FIGURES 1. Well Sampling Locations for the Tutu Wells Site Sampling, Analysis, and Monitoring Plan, St. Thomas, U.S. Virgin Islands. 2. Chlorinated VOC Concentrations for Ramsay Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 3. Chlorinated VOC Concentrations for Tillett Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 4. Chlorinated VOC Concentrations for Eglin n Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 5. Chlorinated VOC Concentrations for Harvey Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 6. Chlorinated VOC Concentrations for LaPlace Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 7. Chlorinated VOC Concentrations for Smith Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. T!~ir oo--* - -•-'' 0205 GERAGHTY & MILLER. INC. FIGURES (Continued) 8. Relative Percent of PCE in Ramsay Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 9. Relative Percent of PCE in Tillett Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 10. Relative Percent of PCE in Eglin H Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 11. Relative Percent of PCE in Harvey Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 12. Relative Percent of PCE in LaPlace Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. 13. Relative Percent of PCE in Smith Well Samples, September 1990 through May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. APPENDIX A. Data Validation Summary Report for the Tutu Wells Site, May 1992 Sampling Event, St. Thomas, U.S. Virgin Islands. TUT 003 O2 06 GERAGHTY <* MILLER. INC SIXTH SAMPLING REPORT MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS INTRODUCTION In April 1990, Geraghty & Miller, Inc. was retained by the Tutu Environmental Investigation Committee (TEIC), which is comprised of Texaco Caribbean Inc. (Texaco) and Esso U.S. Virgin Islands (Esso), to prepare a sampling, analysis, and monitoring plan (SAMP) for the Tutu Wells Site, St. Thomas, U.S. Virgin Islands. This report for the sixth sampling event (May 1992) at the Tutu Wells Site was prepared in accordance with the Administrative Order (AO), effective March 22, 1990, and with the requirements detailed in the "Sampling, Analysis, and Monitoring Plan for Wells, Tutu Wells Site, St. Thomas, U.S. Virgin Islands," prepared in September 1990 (Geraghty & Miller, Inc. 1990). The SAMP was approved by the U.S. Environmental Protection Agency (USEPA) in its September 21, 1990 letter to the TEIC. (USEPA 1990a). The first three ground-water sampling events were performed in September/October 1990, February 1991, and June 1991. Geraghty & Miller and Soil Tech Corporation, Inc. (Soil Tech) of San Juan, Puerto Rico implemented the sampling activities. For each of these three sampling events, Geraghty & Miller prepared reports (Geraghty & Miller, Inc. 1991a, 1991b, and 1991c) that were submitted to the USEPA and the U.S. Virgin Islands Department of Planning and Natural Resources (DPNR). Due to cumulative quality control (QC) problems caused by the previous laboratory, Geraghty & Miller recommended that Enseco East Incorporated (Enseco) of Somerset, New Jersey be retained as the laboratory subcontractor after the third sampling event (Geraghty & Miller, Inc. 1991c). A meeting was held with the USEPA on July 15, 1991 to discuss the new laboratory and to clarify the sampling and analytical procedures. A revised SAMP (Geraghty & Miller, Inc. 1991d), which was submitted to the USEPA in September 1991, incorporated clarifications of the sampling and analytical procedures and included the change in the analytical TUT GERAGHTY & MILLER. INC. 2 laboratory. The revised SAMP (Geraghty & Miller, Inc. 1991d) became effective prior to the fourth sampling event, which took place in October 1991 (Geraghty & Miller, Inc. 1991e). The fifth sampling event was conducted in February 1992 (Geraghty & Miller, Inc. 1992). The objectives of the SAMP (Geraghty & Miller, Inc. 1990) and the revised SAMP (Geraghty & Miller, Inc. 199Id) are to identify, quantify, and monitor the occurrence of gasoline constituents and tetrachloroethene (commonly referred to as perchloroethylene and abbreviated as PCE) and its breakdown products in particular water supply wells in the vicinity of Route 38 within the Tutu Wells Site (see Figure 1). SAMPLING AND ANALYTICAL PROCEDURES The sixth sampling event was conducted from May 27 through 29, 1992 by Soil Tech and Geraghty & Miller. Ms. Ana Gloria Ramos, Designated Coordinator for TEIC, was present throughout the sampling event. Sampling and analysis were performed as described in the revised SAMP (Geraghty & Miller, Inc. 1991d), with the exception of the few deviations outlined later in this section. Table 1 lists the sample locations and analytical parameters for the May 1992 sampling. In brief, the wells were sampled and analyzed for the Target Compound List (TCL) volatile organic compounds (VOCs) in accordance with a modified version of USEPA Method 524.2, Revision 3.0 (USEPA 1989) to achieve lower detection levels. All analyses were performed using contract laboratory protocol (CLP) procedures. Enseco performed the laboratory analyses. TECHNICAL METHODOLOGY All 11 samples (ten wells and one blind replicate) obtained during the May 1992 sampling event were collected utilizing the permanent pumps and piping systems installed in the wells, with the exception of the samples from the Gassett supply well. The Gassett well, which is not equipped with a permanent pump, was purged using a submersible pump powered by a portable TUT O03 0208 GERAGHTY & MILLER. INC. 3 generator. After 1,230 gallons (approximately 4.6 well volumes) were purged from the Gassett well, the submersible pump was removed and a sample was collected using a Teflon bailer. Sample names shown on the tables that require explanation are as follows: • One blind field replicate sample, labelled "Wess," was collected during the sampling event and on the validated data tables was renamed "Smith FR," indicating this sample was a Meld replicate taken from the Smith well. • Matrix spike (MS) and matrix spike duplicate (MSD) samples were collected from the Eglin I well. These samples were labelled "Eglin I MS" and "Eglin I MSD." • On May 27, 1992, the distilled and deionized water provided by Enseco was used to prepare an equipment blank and a water blank. The equipment blank sample was collected by rinsing the distilled and deionized water through the clean Teflon bailer, which was later used to sample the Gassett well. The water blank was collected by pouring the distilled and deionized water from the laboratory- supplied containers into the sample containers. The equipment blank and the water blank were analyzed for TCL VOCs. • The spelling for Harthman was corrected to include the second "h." Trip blank samples were prepared by Enseco and shipped to Soil Tech with the other sample vials. The objective of a trip blank is to measure potential cross-contamination of samples during vial preparation, shipment, and analysis. A trip blank sample (two 40-milliliter vials) was included in each shipment of samples from the Tutu Wells Site to Enseco. Trip blank samples were analyzed for TCL VOCs. Geraghty & Miller validated the analytical data in accordance with the USEPA Standard Operating Procedures (SOP) No. HW-6, January 1992, for organic compounds (USEPA 1992). TUT GERAGHTY & MILLER. INC. 4 The data validation summary is provided in Appendix A. The VOC parameters detected in ground-water samples collected during the sixth sampling event (May 1992) are summarized in Table 2. The complete VOC validated data for the sixth sampling event are presented in Table 3. Details of the sampling and analysis procedures, data validation requirements, and reporting requirements are provided in the revised SAMP (Geraghty & Miller, Inc. 199Id). PROCEDURAL DEVIATIONS Deviations from the scope of work and procedures during the sixth sampling event are explained below. 1. The VIHA I and VIHA n wells were not sampled due to inoperable pumps. 2. Due to the presence of air bubbles in the trip blanks received from Enseco, all trip blank samples were refilled on-site using the distilled, deionized analyte-free water provided by Enseco. 3. The initial Tillett well sample was analyzed within the required holding time. However, the analysis of the Tillett sample secondary dilution, identified as "Tillett DL", was performed 19 days beyond the holding time. Therefore, the reported value of 470 parts per billion (ppb) of total 1,2-dichloroethene (1,2- DCE) was qualified as estimated using the "J" qualifier. Further details are provided in Appendix A. 4. The Four Winds I, Four Winds II, Harthman II, Harthman HI, and Matthias wells were not sampled because the property owners did not allow access. Mr. Sammy Harthman would not allow access to the Harthman property, which is under construction for the proposed Tutu Park/K-Mart Shopping Center. The two Harthman wells are GERAGHTY & MILLER. INC 5 still functional. The Harthman m well (formerly known as the Estate well) is being pumped to supply water for the construction activities. DATA VALIDATION The organic data have been evaluated according to USEPA Region n SOP No. HW-6, Revision No. 8 (USEPA 1992), in conjunction with the USEPA Draft National Functional Guidelines for Organic Data Review (USEPA 1991) and the appropriate corresponding methodology. Because the VOC analyses were not performed in accordance with the CLP Statement of Work (SOW) for organic analysis (USEPA 1990b), the SOP for organic data review is not directly applicable. However the SOP was used, along with USEPA Method 524.2, Revision 3.0 (USEPA 1989) and the additional QC requirements outlined in the revised SAMP (Geraghty & Miller, Inc. 1991d), to conform to the USEPA Region D data validation protocol (USEPA 1992). All of the data have been tabulated and assigned the appropriate qualifier codes, if required. A discussion of the data validation findings is provided in Appendix A. The QC deficiencies are minor therefore, the data are usable with minor qualifications. Sample data have not been rejected when qualified as estimated due to more than one deficiency. All of the organic data generated for the samples are valid and usable. ORGANIC ANALYTICAL RESULTS VOCs were analyzed according to USEPA Method 524.2, Revision 3.0 (USEPA 1989). All VOC analyses were performed within the required holding time, as shown in Table 4, with the exception of the Tillett DL sample, which was reanalyzed with a secondary dilution (DL) 19 days outside the 7-day holding time. Therefore, the result for 1,2-DCE (reported as sum of cis- and trans-isomers) is qualified as estimated using the "J" qualifier. VOCs were detected in various blanks, and associated ground-water samples were qualified as appropriate. Table 5 presents a summary of VOC-contaminated blanks and associated ground-water samples. The TUT 003 0211 GERAGHTY & MILLER. INC 6 complete validated VOC data results for these six sampling events are presented in Table 6. Table 7 presents a summary of detected VOCs for the first six sampling events (September/October 1990, February 1991, June 1991, October 1991, February 1992, and May 1992). In a comparison of applicable or relevant and appropriate requirements with detected analytes in ground water (see Table 8), VOCs were detected at concentrations above the USEPA drinking water standards (see Table 9) in samples collected from the following supply wells: Eglin I, Eglin n, Englin ffl, Harvey, LaPlace, Ramsay, Smith, Steel, and Tillett. VOCs constitute the main group of constituents of concern at the Tutu Wells Site. The compounds that were consistently detected in samples were 1,2-DCE, trichloroethene (TCE), and PCE. PCE was detected in all samples except the Gassett sample. The PCE concentrations ranged from 14 ppb in the Eglin I sample to 350 ppb in the Harvey sample. TCE was detected in all samples, and concentrations range from an estimated concentration of 0.06 ppb in the Gassett sample to 59 ppb in the Tillett sample. 1,2-DCE was detected in all samples except the Gassett sample. The 1,2-DCE concentrations range from 9.5 ppb in the Ramsay sample to an estimated 470 ppb (secondary dilution) in the Tillett sample. The other VOCs detected in the May 1992 sampling event were benzene, bromodichloromethane, chloroform, toluene, and vinyl chloride. Chloroform was detected in seven samples (Eglin I, Eglin II, Eglin ID, LaPlace, Ramsay, Smith, and Tillett) ranging from an estimated concentration of 0.05 ppb in the LaPlace sample to 1.3 ppb in the Ramsay sample. Vinyl chloride was detected in two samples (Steele and Tillett) at concentrations of 2 ppb and 3.2 ppb, respectively. Petroleum constituents such as benzene, toluene, ethylbenzene, and xylenes (BTEX) have not been detected in the majority of the wells. Benzene was detected in two samples (Eglin n and Tillett) at estimated concentrations of 0.07 ppb and 0.8 ppb, respectively. Toluene was detected in two samples (Eglin I and Ramsay) at estimated concentrations of 0.06 ppb and 0.44 ppb, respectively. TUT 003 021: GERAGHTY & MILLER. INC. 7 Only three VOCs (1,2-DCE, TCE, and PCE) have been detected at concentrations above 4 ppb. 1,2-DCE and TCE are potential degradation products of PCE. Graphs showing the concentrations of 1,2-DCE, TCE, and PCE in selected wells from September 1990 through May 1992 are presented on Figures 2 through 7. These graphs illustrate the variation of 1,2-DCE, TCE, and PCE concentrations throughout the six sampling events at the Tutu Wells Site. Of these three chlorinated organic compounds, TCE has generally been detected at the lowest concentration, with 1,2-DCE and PCE usually being reported at higher concentrations than TCE. With the exception of the Ramsay, Harvey, and Smith wells, 1,2-DCE is the VOC that has been present at the highest concentration in wells sampled at the Tutu Wells Site (see Figures 2 through 7). To better evaluate the occurrence of PCE relative to its potential breakdown products, the relative percent of PCE was calculated for analytical results from September 1990 through May 1992 (see Figures 8 through 13). The relative percent of PCE was calculated by dividing the concentration of PCE by the sum of the concentrations of 1,2-DCE, TCE, and PCE. The calculated values for relative percent of PCE are shown in Table 10. The relative percent of PCE at most well locations has been below 45 percent. However, the relative percent of PCE for the Ramsay and Harvey well samples usually exceeded 80 percent (see Figures 8 and 11). The relative percent of PCE for the Smith well samples was between 70 and 85 percent (see Figure 13). For the other wells, shown on Figures 9, 10, and 12, the relative percent of PCE ranged between 20 and 50 percent. Because 1,2-DCE and TCE are potential degradation products of PCE, the high relative percent of PCE at the Ramsay, Harvey, and Smith wells may indicate proximity to a source of PCE. The further the distance downgradient from a PCE source and the more time PCE is exposed to degradation processes in the aquifer, the greater the likelihood that the relative percent of PCE will decrease as PCE is degraded into 1,2-DCE and TCE. GERAGHTY & MILLER. INC. RECOMMENDATIONS The May 1992 sampling results meet the prescribed objectives of the revised SAMP (Geraghty & Miller, Inc. 1991d). Geraghty & Miller recommends that the revised SAMP (Geraghty & Miller, Inc. 199Id) continue to be followed, but that the revisions discussed below be implemented. • The seventh sampling event (scheduled to begin on September 14, 1992) should include analysis for only TCL VOCs, using USEPA Method 524.2 Revision 3.0 (USEPA 1989) following CLP protocol. • The seventh sampling event should only include the wells listed in Table 11. TUT 003 0214 GERAGHTY & MILLER. INC. REFERENCES Geraghty & Miller, Inc. 1990. Sampling, Analysis, and Monitoring Plan for Wells, Tutu Wells Site, St. Thomas, U.S. Virgin Islands, September 1990. Geraghty & Miller, Inc. 199la. First Sampling Report, September 1990, Tutu Wells Site Quarterly Sampling, St. Thomas, U.S. Virgin Islands, January 1991. Geraghty & Miller, Inc. 1991b. Second Sampling Report, February 1991, Tutu Wells Site Quarterly Sampling, St. Thomas, U.S. Virgin Islands, May 1991. Geraghty & Miller, Inc. 1991c. Third Sampling Report, June 1991, Tutu Wells Site Quarterly Sampling, St. Thomas, U.S. Virgin Islands, September 1991. Geraghty & Miller, Inc. 199 Id. Revised Sampling, Analysis, and Monitoring Plan for Wells, Tutu Wells Site, St. Thomas, U.S. Virgin Islands, September 1991. Geraghty & Miller, Inc. 1991e. Fourth Sampling Report, October 1991, Tutu Wells Site, St. Thomas, U.S. Virgin Islands, January 1992. Geraghty &, Miller, Inc. 1992. Fifth Sampling Report, February 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands, May 1992. U.S. Environmental Protection Agency (USEPA). 1989. Method 524.2, Revision 3.0, Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectroscopy, Environmental Monitoring Systems Laboratory (EMSL), Office of Research and Development. U.S. Environmental Protection Agency (USEPA). 1990a. Letter Correspondence from Carole Petersen, USEPA Chief New York/Caribbean Compliance Branch, to Ana Gloria Ramos, Designated Coordinator, Tutu Environmental Investigation Committee, September 21, 1990. U.S. Environmental Protection Agency (USEPA). 1990b. USEPA Contract Laboratory Program, Statement of Work for Organic Analysis, Multi-Media, Multi-Concentration, SOW No. 3/90 including Rev. 12/90 and 2/91, March 1990. U.S. Environmental Protection Agency (USEPA). 1991. Draft National Functional Guidelines for Organic Data Review, Multi-Media, Multi-Concentration (OLM01.0), December 1990, revised June 1991. 02 GERAGHTY & MILLER. INC 10 REFERENCES (Continued) U.S. Environmental Protection Agency (USEPA). 1992. Contract Laboratory Program (CLP) Organics Data Review and Preliminary Review, Region n Standard Operating Procedure No. HW-6, Revision No. 8, January 1992. U.S. Geological Survey (USGS). 1954. Eastern St. Thomas, Virgin Islands. 7.5-minute Topographic Quadrangle Map. MR:nna IPROOSOlHTC/Sixth.qtr TUT 003 0216 GERAGHTY & MILLER. INC. Table 1. List of Sample Locations and Analytical Parameters for the Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Sample ID Proposed Analytes Eglin I Eglin II Eglin ffl Gassett Harvey LaPlace Ramsay Smith Steele Tillett TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL VOCs TCL Target compound list. VOCs Volatile organic compounds. VOC analysis was performed using modified USEPA Method 524.2, Revision 3.0 (USEPA 1989). TD:ce/rma (TPR0080I -vT2y6ttiqtr.fi* GERAGHTY & MILLER. INC Table 2. Summary of Detected Volatile Organic Compounds in Ground-Water Samples Collected in May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Page 1 of 2 Sample ID: Analyte Date: Vinyl chloride Meuylene chloride 1 ,2-Dichloroethene (cis/trans) Chloroform Bromodichloromethane Trichloroethene Benzene Tetrachloroethene Toluene EglinI 27-May-92 ND ND 13 0.05 J ND 6.3 ND 14 0.06 J EglinH 27-May-92 ND ND 31 0.09 J ND 14 0.07 J 36 ND Eglinm 28-M«y-92 ND ND 31 0.07 J ND 14 ND 39 ND GMtett 27-Mty-92 ND ND ND ND ND 0.06 J ND ND ND Harvey 28-M«y-92 ND ND 41 ND ND 29 ND 350 ND La Place 28-May-92 ND ND C10 ., I CHECKED: REIVE I APPROVED: DANAHY I DRAFTER: NU_.« 25-r 20-- 10/1/90 2/5/91 LEGEND PCE TETRACHLOROETHENE 1.2-DCE DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE VOC VOLATILE ORGANIC COMPOUND ppb PARTS PER BILLION 7/15/92 6/5/91 10/1/91 D A T E 5/28/92 GERAGHTY & MILLER, INC. Environmental Services CHLORINATED VOC CONCENTRATIONS FOR RAMSAY WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS FIGURE IDWG( £: 8/13/92 I PRJCT NO.: PR01301 I FILE NO.: TU-54 I DRAWNG: TU-\. I CHECKED: REIVE (APPROVED: DANAHY I OR AFTER: NIXO., 10/2/90 PCE 1.2-DCE TCE VOC ppb LEGEND TETRACHLOROETHENE DICHLOROETHENE (TOTAL) TRICHLOROETHENE VOLATILE ORGANIC COMPOUND PARTS PER BILLION 2/5/91 6/5/91 10/2/91 D A T E 7/15/92 5/29/92 GERAGHTY & MILLER, INC. Environmental Services CHLORINATED VOC CONCENTRATIONS FOR TILLETT WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS. U.S. VIRGIN ISLANDS FIGURE IDWGV .: 8/13/92 I PRJCT NO.: PR01301 I FILE NO.: TU-55 IDRAWNG: TU-l I CHECKED: REIVE [APPROVED: DANAHY I DRAFTER: NIXL 140-r 120 -- 100 -- 80-- 60-- 40-- 20-- PCE 1.2-DCE TCE VOC ppb LEGEND TETRACHLOROETHENE OICHLOROETHENE (TOTAL) TRICHLOROETHENE VOLATILE ORGANIC COMPOUND PARTS PER BILLION 8/15/00 1/1/91 9/27/90 2/5/91 6/5/91 10/2/91 D A T E 1/1/92 2/3/92 7/15/92 5/27/92 GERAGHTY & MILLER, INC. Environmental Services CHLORINATED VOC CONCENTRATIONS FOR EGUN II WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS. U.S. VIRGIN ISLANDS FIGURE I: 8/13/92 | PRJCT NO.: PR01301 I RLE NO.: TU-52 IDRAVWNG: TUi [CHECKED: REIVE I APPROVED: OANAHY I DRAFTER: NIXo.« 1600-- 1400-- O 1200 -- 1000 -- 800 -- 600 -- 400-- 200-- pee LEGEND PCE TETRACHLOROETHENE 1.2-DCE DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE VOC VOLATILE ORGANIC COMPOUND ppb PARTS PER BILLION 2/5/91 6/4/91 10/2/91 D A T E 1/1/92 2/3/92 5/28/92 GERAGHTY & MILLER, INC. Environmental Services CHLOFMNATED VOC CONCENTRATIONS F=OR HARVEY WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS FIGURE ": 8/13/92 | PRJCT NO.: PR01301 [ RLE NO.: 711-56 [DRAWNG: TU-( | CHECKED: REIVE I APPROVED: DANAHY | DRAFTER: Nl 250 -r 200 -- 150 -- 100-- 50-- LEGEND PCE TETRACHLOROETHENE 1.2-DCE DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE VOC VOLATILE ORGANIC COMPOUND ppb PARTS PER BILLION 1,2-DCE TCE 8/15/90 1/1/91 10/2/90 2/5/91 1/1/92 6/6/91 10/3/91 D A T E 2/6/92 7/15/82 5/28/92 GERAGHTY JilT & MILLER, INC. Environmental Services CHLORINATED VOC CONCENTRATIONS FOR LAPLACE WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS. U.S. VIRGIN ISLANDS FIGURE [DWo( E: 6/13/92 | PRJCT NO.: PRO!301 I FILE NO.: TU-57 I DRAWING: TU\ I CHECKED: REIVE (APPROVED: DANAHY I DRAFTER:: NIA*, 350 -T- 300 -- 250 -- 200 -- 150 -- 100-- 50-- B/ 5/00 9/25/90 1/1/91 LEGEND PCE TETRACHLOROETHENE 1.2-DCE OICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE VOC VOLATILE ORGANIC COMPOUND ppb PARTS PER BILLION X2-DCE PCE 2/5/91 1/1/82 6/6/91 10/3/91 2/5/92 D A T E 7/15/92 5/28/92 GERAGHTY & MILLER, INC. Environmental Services CHLORINATED VOC CONCENTRATIONS FOR SMITH WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS FIGURE T: 8/13/92 IPRJCT NO.: PR00801 I FILE NO.: TU-5B IDRAYWNG: TU-( I CHECKED: REIVE [APPROVED: DANAHY I DRAFTER: 100%-r- 90%-- 80%-- 70%-- 60%-- 50%-- 40%-- 30%-- 20% - - 10%-- 0% e/is/90 RELATIVE PERCENT OF PCE LEGEND [PCE] [1.2-DCE] + [TCE] + [PCE] CONCENTRATION OF TCE TETRACHLOROETHENE 1,2-DICHLOROETHENE (TOTAL) TRICHLOROETHENE 1/1/91 10/1/90 2/5/91 6/5/91 10/1/91 D A T E 1/1/92 2/4/92 7/15/92 5/28/92 GERAGHTY & MILLER, INC. Environmental Services RELATIVE PERCENT OF PCE IN RAMSAY WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS FIGURE 8 I DWGV J: 8/13/92 [ PRJCT NO.: PR00801 I RLE NO.: UI-59 I DRAWING: TU-1 I CHECKED: REIVE I APPROVED: DANAHY I DRAFTER: 100%-, 90%- m 80*- ft70"' t 60%- Q 50%- m 40X" J ^" 30%- 20%- 10%- 8/1 1 LEGEND RELATIVE [PCE] PERCENT OF PCE [i,2-OCE] + [TCE] + [PCE] [TCE] CONCENTRATION OF TCE PCE TETRACHLOROETHENE 1.2-DCE 1.2-DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE ^^^^^ B________—— -—— ———— ——— ——— -____ _____________ w^^ ^\. ————— | ————————— , —————— | ——————————————— | ——————————————— | ——————————— , ———— | —————————————— | —————— | 5/90 1/1/91 1/V92 7/15/92 10/2/90 2/5/91 6/6/91 10/2/91 2/5/92 5/29/92 D A T E i AW GERAGHTY RELATIVE PERCENT OF PCE IN TILLETT WELL SAMPLES FIGURE £& & MILLER. INC. SEPTEMBER 1990 THROUGH MAY 1992 ^ Environmental Servic.5 TUJU ^^ ^£ 9 ' ———————————————————— ST. THOMAS, U.S. VIRGIN ISLANDS C • J -: 8/13/92 | PRJCT NO.: PR00801 [RLE NO.: TU-60 I DRAWNG: TU-l I CHECKED: REIVE [APPROVED: DANAHY I DRAFTER: NIXt 100%T 90%-- 60%-- 50%-- 30%-- 20%-- 10%-- RELAT1VE PERCENT OF PCE [TCE] PCE 1.2-DCE TCE LEGEND [PCE] 11.2-DCE] + [TCE] + [PCE] CONCENTRATION OF TCE TETRACHLOROETHENE 1.2-DICHLOROETHENE (TOTAL) TRICHLOROETHENE 8/15/90 1/1/91 9/27/90 2/5/91 6/5/91 10/2/91 D A T E 1/1/92 2/3/92 7/15/92 5/27/92 GERAGHTY & MILLER, INC. Jrnvironnu,^ Services RELATIVE PERCEm" OF PCE IN EGLIN II WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU ST. THOMAS. U.S. VIRGIN ISLANDS FIGURE 10 DWG t -: 8/13/92 | PRJCT NO.: PR00801 I RLE NO.: TU-61 IDRAWNG:!: TU-fi. I CHECKED: REIVE (APPROVED: DANAHY I DRAFTER: NIXO.. 100% -r- 90%-- 60%-- 50%-- 40%-- 20%-- 10%-- RELATIVE PERCENT OF PCE [TCE] PCE 1.2-DCE TCE LEGEND [PCE] [1.2-OCE] + [TCE] -I- [PCE] CONCENTRATION OF TCE TETRACHLOROETHENE 1.2-WCHLOROETHENE (TOTAL) TRICHLOROETHENE 8/15/90 9/26/90 1/1/91 2/5/91 6/4/91 10/2/91 1/1/92 2/3/92 7/15/92 5/28/92 D A T E GERAGHTY & MILLER, INC. RELATIVE PERCENT OF PCE IN HARVEY WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 FIGURE ST. THOMAS, U.S. VIRGIN ISLANDS |DWa £: 8/11/92 | PRJCT NO.: PROOB01 I RLE NO.: TU-62 I DRAWING: TUA. I CHECKED: REIVE I APPROVED: OANAHY I DRAFTER:!: NIXv. RELATIVE LEGEND [ pCE] PERCENT OF PCE [1.2-OCE] + [TCE] + [PCE] [TCE] CONCENTRATION OF TCE PCE TETRACHLOROETHENE 1,2-DCE 1.2-DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE 8/15/90 1/1/91 10/2/90 2/5/91 1/1/92 6/6/91 10/3/91 D A T E 2/6/92 7/15/92 5/28/92 GERAGHTY & MILLER, INC. Environmental Services RELATIVE PERCENT OF PCE IN LAPLACE WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS, U.S. VIRGIN ISLANDS FIGURE 12 I DWG i B/11/92 I PRJCT NO.: PROOB01 | FILE NO.: TU-63 [DRAWING: TU-6V | CHECKED: REIVE [APPROVED: DANAHY | DRAFTER: NIXO> RELATIVE LEGEND [PCE] PERCENT OF PCE [1,2-DCE] + [TCE] + [PCE] [TCE] CONCENTRATION OF TCE PCE TETRACHLOROETHENE 1.2-DCE 1.2-DICHLOROETHENE (TOTAL) TCE TRICHLOROETHENE B/15/90 1/1/91 9/25/90 2/5/91 1/1/92 6/6/91 10/3/91 D A T E 2/5/92 7/15/92 5/28/92 GERAGHTY & MILLER, INC. Environmental Services RELATIVE PERCENT OF PCE IN SMITH WELL SAMPLES SEPTEMBER 1990 THROUGH MAY 1992 TUTU WELLS SITE ST. THOMAS. U.S. VIRGIN ISLANDS FIGURE 13 APPENDIX A DATA VALIDATION SUMMARY REPORT FOR THE TUTU WELLS SITE MAY 1992 SAMPLING EVENT ST. THOMAS, U.S. VIRGIN ISLANDS GERAGHTY & MILLER. INC. APPENDIX A DATA VALIDATION SUMMARY REPORT FOR THE TUTU WELLS SITE, MAY 1992 SAMPLING EVENT, ST. THOMAS, U. S. VIRGIN ISLANDS Appendix A includes the data validation summary report and supporting documentation generated during the analytical data review of ground-water samples collected from May 27 through 29, 1992 at the Tutu Wells Site, St. Thomas, U.S. Virgin Islands. APPENDIX FORMAT The data validation report appendix is divided into the following sections: • Introduction. • Attachment No. 1 - The U.S. Environmental Protection Agency (USEPA) Standard Operating Procedure (SOP) Number (No.) HW-6 (Revision No. 8) Contract Laboratory Program (CLP) organics preliminary data review checklist, the data assessment narrative, and the organic regional data assessment form. • Attachment No. 2 - Tables associated with the data validation assessment narrative. • Attachment No. 3 - Analytical data packages. The introduction summarizes (1) the field investigation sampling effort, (2) the analytical parameters and methods employed in support of the field investigation, and (3) the data validation requirements and validation protocols used for the data assessment. Attachment No. 1 is comprised of the USEPA SOP No. HW-6 (Revision No. 8) CLP organics preliminary data review checklist, the data assessment narrative, and the organic regional data assessment form (USEPA 1992). The data review checklist guides the data reviewer in evaluating pertinent field and laboratory sample documentation and analytical procedures. By evaluating critical quality control (QC) criteria, the data reviewer determines the validity of generated data and places limitations on data use. In the data assessment GERAGHTY & MILLER. INC A-2 narrative, the data reviewer summarizes the validation, discusses sample anomalies and QC outliers, and provides an overall assessment of the analytical data generated in support of the field investigation. The organic regional data assessment form provides a condensed data assessment summary. In Attachment No. 2, tabulated data is provided which summarizes any holding time non- compliance; associated trip blank, equipment blank, and method blank contamination; laboratory fortified blank (LFB) QC exceedances; and validated analytical data with applied qualifiers. Attachment No. 3 is comprised of the analytical data packages prepared by the laboratory for all samples collected and reviewed for this field investigation. They are available upon request. GERAGHTY c> MILLER. INC A-3 INTRODUCTION This report presents the data validation and narrative summary for the following 11 ground-water samples, one equipment blank, and three trip blanks collected in May 1992 at the Tutu Wells Site, St. Thomas, U.S. Virgin Islands: Enseco-East Project Numbers Sample Identifiers Collection Date 22277 Eglin I, Eglin II, Steele, Gassett, 5/27/92 Equipment Blank, Trip Blank (5/27/92). 22312 Harvey, Ramsay, Eglin III, Smith, 5/28/92 Wess (field replicate [FR] of Smith), LaPlace, Trip Blank (5/28/92). 22352 Tillett, Trip Blank (5/29/92). 5/29/92 All of the samples were analyzed for target compound list (TCL) volatile organic compounds (VOCs). In addition, a library search was performed for ten tentatively identified compounds (TICs) using comparison of sample spectra against the reference library mass spectra. Sample analyses were performed by Enseco-East (Enseco), a laboratory division of Enseco Incorporated located in Somerset, New Jersey. VOCs were analyzed according to USEPA Method 524.2, Revision 3.0 (USEPA 1989). The organic data have been evaluated according to USEPA Region II SOP No. HW-6, Revision No. 8 (USEPA 1992), in conjunction with the USEPA Draft National Functional Guidelines for Organics Data Review (USEPA 1991) and the appropriate, corresponding methodology. Because the VOC analyses were not performed in accordance with the CLP statement of work (SOW) (USEPA 1990), the SOP for organic data review is not directly applicable. The SOP was used along with USEPA Method 524.2, Revision 3.0 (USEPA 1989) GERAGHTY & MILLER. INC A-4 and the additional QC requirements outlined in the revised Sampling, Analysis, and Monitoring Plan (SAMP) (Geraghty & Miller, Inc. 1991), to conform to the USEPA Region II data validation protocol (USEPA 1992). All of the data have been tabulated and assigned the appropriate qualifier codes, if required. The validated data table is provided as Table A-4 in Attachment No. 2. TUT GERAGHTY & MILLER. INC A-5 REFERENCES Geraghty & Miller, Inc. 1991. Revised Sampling, Analysis, and Monitoring Plan for Wells, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Prepared for Tutu Environmental Investigation Committee, September 1990, revised September 1991. U.S. Environmental Protection Agency (USEPA). 1989. Method 524.2, Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectroscopy, Revision 3.0. Environmental Monitoring Systems Laboratory (EMSL), Office of Research and Development, United States Environmental Protection Agency, 1989. U.S. Environmental Protection Agency (USEPA). 1990. USEPA Contract Laboratory Program, Statement of Work for Organic Analysis, Multi-Media, Multi-Concentration, SOW No. 3/90 including Rev. 12/90 and 2/91, United States Environmental Protection Agency, March 1990. U.S. Environmental Protection Agency (USEPA). 1991. Draft National Functional Guidelines for Organic Data Review, Multi-Media, Multi-Concentration (OLMOI.O), United States Environmental Protection Agency, December 1990, revised June 1991. U.S. Environmental Protection Agency (USEPA). 1992. Contract Laboratory Program (CLP) Organics Data Review and Preliminary Review, Region II Standard Operating Procedure No. HW-6, Revision No. 8, United States Environmental Protection Agency, January 1992. PR00801-DV2/592INTRO TUT 003 0276 GERAGHTY ^ MILLER. INC ATTACHMENT NO. 1 U.S. ENVIRONMENTAL PROTECTION AGENCY STANDARD OPERATING PROCEDURE NO. HW-6 REVISION NO. 8 TUT GERAGHTY & MILLER. INC. SOP NO. HW-6 Revision 18 CLP ORGANICS DATA REVIEW AND PRELIMINARY REVIEW BY: - Leon Lazarus, Environmental Scientist Tox±3 and Hazardous Waste Section BY: ffeorge Kafrras, Chemist Toxic and Hazardpus Waste Section BY: ______________ •''•£•' •'-'-•~)_______ Stelios Gerazounis/ Chemist Toxic and Hazardous Waste Section CONCURRED BY: Kevin Rub md APPROVED BY: Date: L/ Date: //£ Date: s Waste Section Robert Runyon, Chief Monitoring Management Branch Date: STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review and Preliminary Review Page 1 of 61 Date: January 1992 Number HW-6 Revision: 8 PACKAGE COMPLETENESS AND DEIJVERABLES CASE NUMBER:22277. 22312. 22352___________ SITE: Tutu Wells 1.0 DATA COMPLETENESS AND DELIVERABLES 1.1 Have any missing deliverables been received and added to the data package? ACTION; Call lab for explanation/resubmittal of any missing deliverables. If lab cannot provide them, note the effect on review of the package under the "Contract Problems/Non-Compliance11 section of reviewer narrative. 1.2 Was SMO CCS checklist included with package? 2.0 COVER LETTER SDG NARRATIVE 2.1 Is the Narrative or Cover Letter Present? 2.2 Are Case Number and/or SAS number contained in the Narrative or Cover letter? 3.0 DATA VALIDATION CHECKLIST The following checklist is divided into three parts. Pan A is filled out if the data package contains any VOA analyses, Part B for any BNA analyses and Part C for Pesticide/PCBs. YES NO N/A LAB: Enseco-East UU UU STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review and Preliminary Review Page 2 of 61 Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 3.0 DATA VALIDATION CHECKLIST (continued) Does this package contain: VOA Data? BNA Data? Pesticide/PCB data? ACTION; Complete corresponding parts of checklist. PART A: VOA ANALYSES 1.0 TRAFFIC REPORTS AND LABORATORY NARRATIVE 1.1 Are the Traffic Report Forms present for all samples? ACTION; If no, contract lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special circumstances affecting the quality of the data? ACTION; If any sample analyzed as a soil, other than TCLP, contains 50%-90% water, all data should be flagged as estimated (J). If a soil sample other than TCLP contains more than 90% water, all data should be qualified as unusable (R). ACTION: If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all Non-Detects "UJ". UL1 TUI STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 3 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: If both VOA vials for a sample have air bubbles or the VOA vial analyzed had air bubbles, flag all positive results "J" and all non-detects "R". 2.0 HOLDING TIMES 2.1 Have any VOA technical holding times, determined from date of collection to date of analysis, been exceeded? X [_] __ If unpreserved, aqueous samples maintained at 4°C which are to be analyzed for aromatic hydrocarbons must be analyzed within 7 days of collection. If preserved with HC1 (pH<2) and stored at 4°C, then aqueous samples must be analyzed within 14 days of collection. If uncertain about preservation, contact sampler to determine whether or not samples were preserved. The holding time for soils is 10 days. Table of Holding Time Violations (See Narrative) Sample Sample Date Date Lab Date ID Matrix Preserved? Sampled Received Analyzed TU" STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 4 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If technical holding times ar exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon re-analysis, the reviewer must use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results must be qualified "J", but the reviewer may determine that non-detect data are unusable (R). If holding times are exceeded by more than 28 days, all non detect data are unusable (R). 3.0 System Monitoring Compound (SMO Recovery (Form II) 3.1 Are the VOA SMC Recovery Summaries (Form II) present for each of the following matrices: a. Low Water [ X] b. Low Soil [__] c. Med Soil [__] 3.2 Are all the VOA samples listed on the appropriate System Monitoring Compound Recovery Summary for each of the following matrices: a. Low Water [ X] b. Low Soil [__] c. Med Soil [__] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 5 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.3 Were outliers marked correctly with an asterisk? [__] __ X ACTION; Circle all outliers in red. 3.4 Was one or more VOA system monitoring compound recovery outside of contract specifications for any sample or method blank? __ [ X ] If yes, were samples re-analyzed? [__] __ Were method blanks re-analyzed? [__] __ ACTION; If recoveries are > 10% but 1 or more compounds fail to meet SOW specifications: 1. All positive results are qualified as estimated (J). 2. Flag all non-detects as estimated detection limits ("UJ") where recovery is less than the lower acceptance limit 3. If SMC recoveries are above allowable levels, do not qualify non-detects. If any system monitoring compound recovery is <10%: 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as unusable ("R"). STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 6 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A Professional judgement should be used to qualify data that only have method blank SMC recoveries out of specification in both original and re-analyses. Check the internal standard areas. 3.5 Are there any transcription/calculation errors between raw data and Form D? __ [ X] __ ACTION; If large errors exist, call lab for explanation/resubmittal, make any necessary corrections and not errors in the data assessment. 4.0 Matrix Spikes (Form IIP 4.1 Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form m) present? [ X] __ __ 4.2 Were matrix spikes analyzed at the required frequency for each of the following matrices: a. Low Water [ X] __ __ b. Low Soil [__] __ X c. MedSoil [__] __ X ACTION; If any matrix spike data are missing, take the action specified in 3.2 above. 4.3 How may VOA spike recoveries are outside QC limits? Water Soils 0_ out of 10 N/A out of 10 02BA STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 7 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 4.4 How may RPD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? Soils N/A out of 5 ACTION! No action is taken based on MS/MSD data alone. However, using informed professional judgement, the MS/ MSD results may be used in conjunction with other QC criteria to determine the need for qualification of the data. 5.0 Blanks (Form TV) 5.1 Is the Method Blank Summary (Form IV) present? [ X ] __ __ 5.2 Frequency of Analysis: for the analysis of VOA TCL compounds, has a reagent/method blank been analyzed for each SDG or every 20 samples of similar matrix (low water, low soil, medium soil), whichever is more frequent? [ X ] __ __ 5.3 Has a VOA method/instrument blank been analyzed at least once every twelve hours for each concentration level and GC/MS system used? [ X ] __ __ ACTION; If any method blank data are missing, call lab for explanation/resubmittal. If method blank data are not available, reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank or trip blank data for missing method blank data. TUT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 8 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 5.4 Chromatography: review the blank raw data - chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for VOAs? [ X ] ACTION: Use professional judgement to determine the effect on the data. 6.0 Contamination NOTE; "Water Blanks", "drill blanks", and distilled water blanks" are validated like any other sample, and are not used to qualify data. Do not confuse them with the other QC blanks discussed below. 6.1 Do any method/instrument/reagent blanks have positive results (TCL and/or TIC) for VOAs? When applied as describe below, the contaminant concentration in these blanks are multiplied by the sample dilution factor and corrected for % moisture when necessary. X [__] 6.2 Do any field/trip/rinse blanks have positive VOA results (TCL and/or TIC)? X [__] ACTION: Prepare a list of the sample associated with each of the contaminated blanks. (Attach a separate sheet). NOTE; All field blank results associated to a particular group of samples (may exceed one per case) must be used to qualify data. Trip blanks are used to qualify only those samples with which they were shipped and are not required for non-aqueous matrices. Blanks may not be qualified STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review and Preliminary Review Page 9 of 61 Date: January 1992 Number HW-6 Revision: 8 because of contamination in another blank. Field blanks & Trip blanks must be qualified for system monitoring compound, instrument performance criteria, spectral or calibration QC problems. ACTION; Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If any blanks are grossly contaminated, all associated data should be qualified as unusable (R). YES NO N/A Sample cone > CRQL but < 10 x blank value Sample cone < CRQL & < lOx blank value Sample cone > CRQL & > lOx blank value Methylene Flag sample result with Chloride a "U" Acetone Toluene 2-Butanone Sample cone > CRQL but < 5x blank Report CRQL & qualify "U" No qualification is needed Sample cone < CRQL Sample cone > CRQL & is < 5x blank value value & > 5x blank value Other Flag sample result Contam- with a "U" inants Report CRQL & qualify No qualification is "U" needed NOTE; Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 10 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable) 6.3 Are there field/rinse/equipment blanks associated with every sample? [ X ] __ __ ACTION; For low level samples, note in data assessment that there is no associated field/rinse/equipment blank. Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 GC/MS Instrument Performance Check (Form V) 7.1 Are the GC/MS instrument Performance Check Forms (Form V) present for Bromofluorobenzene (BFB)? [ X] 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the BFB provided for each twelve hour shift? [ X] 7.3 Has an instrument performance compound been analyzed for every twelve hours of sample analysis per instrument? [ X ] ACTION; List date, time, instrument ID, and sample analysis for which no associated GC/MS tuning data are available. TUT STANDARD OPERATING PROCEDURE Title: CLP Organic* Data Review Page 11 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION; If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. 7.4 Have the ion abundances been normalized to m/z 95? [ X ] __ ACTION; If mass assignment is in error, qualify all associated data as unusable (R). 7.5 Have the ion abundance criteria been met for each instrument used? [ X ] __ ACTION; List all data which do not meet ion abundance criteria (attach a separate sheet). ACTION; If ion abundance criteria are not met, the Region n TPO must be notified. 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? (Check at least two values but if errors are found, check more). __ [ X ] 7.7 Have the appropriate number of significant figures (two) been reported? [ X ] __ TUT 005 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review and Preliminary Review Page 12 of 61 Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 7.8 Are the spectra of the mass calibration compound acceptable? 8.0 Target Compound List (TCP Analytes 8.1 Are the Organic Analysis Data Sheets (Form I VOA) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate b. Matrix spikes and matrix spike duplicates c. Blanks UU _ UU UU _ 8.2 Are the VOA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following? a. Samples and/or fractions as appropriate UU _ b. Matrix spikes and matrix spike duplicates (Mass spectra not required [_] c. Blanks [ X] ACTION! If any data are missing, take action specified in 32 above. 8.3 Are the response factors shown in the Quant Report? [__] X STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 13 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 8.4 Is chromatographic performance acceptable with respect to: Baseline stability? [ X ] __ __ Resolution? [ X] __ __ Peak shape? [ X] __ __ Full-scale graph (attenuation)? [ X ] __ __ Other: ___________ [__] __ _JL_ ACTION: Use professional judgement to determine the acceptability of the data. 8.5 Are the lab-generated standard mass spectra of the identified VOA compounds present for each sample? [ X ] ACTION; If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problems/Non-compliance". 8.6 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? [ X J 8.7 Are all ions present in the standard mass spectrum at a relative intensity greater than 10% also present in the sample mass spectrum? [ X ] 8.8 Do sample and standard relative ion intensities agree within 20%? [ X] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 14 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; Use professional judgement to determine acceptability of data. If it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in 8.6, 8.7, and 8.8. ACTION; When sample carry-over is a possibility, professional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIP 9.1 Are all Tentatively Identified Compound Forms (Form I Part B) present; and do listed TICS include scan number or retention time, estimated concentration and "JN" qualifier? [__] X __ 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate [ X ] __ __ b. Blanks [ X] __ __ ACTION; If any TIC data are missing, take action specified in 3.2 above. ACTION; Add "JN" qualifier if missing. TUT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 15 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 93 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2-dimethylbenzene is xylene-a VOA TCL analyte - and should not be reported as a TIC)? __ [ X] __ ACTION; Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity grater than 10% also present in the sample mass spectrum? [ X ] __ __ 9.5 Do TIC and "best match" standard relative ion intensities agree within 20%? [ X ] __ __ ACTION; Use professional judgement to determine acceptable of TIC identifications. If it is determined that an incorrect identification was made, change identification to "unknown" or to some less specific identification (example: "C3 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is detected in a sample and is a suspected artifact of a common laboratory contaminant, the result should be qualified as unusable (R). (i.e. Common Lab Contaminants: Co2 (M/E 44), Siloxanes (M/E 73) Hexane, Aldol Condensation Products, Solvent Preservatives, and related by products - see Functional Guidelines for more guidance). "UT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 16 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 10.0 Compound Ouantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Verity that the correct internal standard, quantitation ion, and RRF were used to calculate Form I result. Were any errors found? __ [ X ] 10.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, sample moisture? [ X ] __ ACTION; If errors are large, call lab for explanation/ resubmittal, make any necessary corrections and note errors under "Conclusions". ACTION: When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and its associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form I's that should not be used, including any in the summary package. 11.0 Standards Data CGC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant. Reports) present) for initial and continuing calibration? [ X ] O2V4 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 17 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (Form VD 12.1 Are the Initial Calibration Forms (Form VI) present and complete for the volatile fraction at concentrations 10, 20, 50, 100, 200 ug/1? Are there separate calibrations for low water/med soils and low soil samples? [_] __ ACTION; If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Were all low level soil standards, blanks and samples analyzed by heated purge? [_] __ ACTION; If low level soil samples were not heated during purge, qualify positive hits "J" and non-detects "R". 12.3 Are response factors stable for VGA's over the concentration range of calibration (% Relative Standard Deviation (%RSD) <30.0%)? [ X] __ ACTION; Circle all outliers in red. NOTE; Although 11 VOA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. ACTION; If %RSD > 30.0%, qualify associated positive results for that analyte T and non-detects using professional judgement. When RSD > 90%, flag all non-detects for that analyte R (unusable). TIT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 18 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A NOTE; Analytes previously qualified TJ" for blank contamination are still considered as "hits" when qualifying for initial calibration criteria. 12.4 Are the RRFs above 0.05? [_] X __ ACTION; Circle all outliers in red. ACTION; If any RRF are < 0.05, qualify associated non-detects (R) and flag associated positive data as estimated (J). 12.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or %RSD? (check at least 2 values, but if errors are found, check more). __ [ X ] __ 13.0 GC/MS Continuing Calibration (Form VII) 13.1 Are the Continuing Calibration Forms (From VII) present and complete for the volatile fraction? [ X ] __ __ 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? [ X ] __ __ ACTION; List below all sample analyses that were not within twelve hours of the previous continuing calibration analysis. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 19 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/ resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). 13.3 Do any volatile compounds have a % Difference (%D) between the initial and continuing RRF which exceeds the ± 25% criteria? X [__] __ ACTION; Circle all outliers in red. ACTION; Qualify both positive results and non-detects for the outlier compound(s) as estimated. When % D is above 90%, reject all non-detects for that analyte (R) unusable. 13.4 Do any volatile compounds have a RRF <0.05? X [_] __ ACTION; Circle all ouliers in red. ACTION; If the RRF <0.05, qualify associated non-detects as unusable (R) and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % difference (%D) between initial and continuing RRFs? (Check at least two values but if errors are found, check more.) __ [ X ] __ ACTION; Circle errors in red. ACTION; If errors are large, call lab for explanation/resubmittal, make any necessary corrections and note errors under "Conclusions". STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 20 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 14.0 Internal Standard (Form Vim 14.1 Are the internal standard areas (From VIE) of every sample and blank within the upper and lower limits (-50% to +100 %) for each continuing calibration. [ X ] __ __ ACTION; List all the outliers below. Sample # Internal Std Area Lower Limit Upper Limit (Attach additional sheets if necessary). ACTION; 1. If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results quantitated with this internal standard. 2. Non-detects associated with IS area counts > 100% should not be qualified. 3. If IS area is below the lower limit (<50%), qualify all associated non-detects (U values) "J". If extremely low area counts are reported, (<25% or if performance exhibits a major abrupt drop off, flag all associated non-detects as unusable ("R"). STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 21 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 14.2 Are the retention times of the internal standards within 30 seconds of the associated calibration standard? [ X ] __ __ ACTION; Professional judgement should be used to qualify data if the retention times differ by more than 30 seconds. 15.0 Field Duplicates 15.1 Were any field duplicates submitted for VOA analysis? [ X ] __ __ ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTION; Any gross variation between duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. #PR00801DV3/7920RGAN.DTA STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 22 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 PARTB; BNA ANALYSES YES NO N/A 1.0 Traffic Reports and Lflfrffpitorv Narrative 1.1 Are the Traffic Report Forms present for all samples? [__] __ __ ACTION; If no, contact lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or Lab Narrative indicate any problems with sample receipt, condition of samples, analytical problems or special notations affecting the quality of the data? __ [__] ACTION; If any sample analyzed as a soil, other than TCLP, contains 50%-90% water, all data should be flagged as estimated ("J"). If a soil sample, other than TCLP, contains more than 90% water, all data should be qualified as usable (R). ACTION; If samples were not iced upon receipt at the laboratory, flag all positive results "J" and all non-detects "UJ". 2.0 Holding Times 2.1 Have any BNA technical holding times, determined from date of collection to date of extraction, been exceeded? __ [__] Continuous extraction of water samples for BNA analysis be started within seven days of the date of collection. Soil/sediment samples must be extracted within 7 days of collection. Extracts must be analyzed within 40 days of the date of extraction. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 23 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A Table of Holding Time Violations (See Narrative) (See Traffic Report) Sample Date Date Lab Date Date Sample Matrix Stamped Received Extracted Analyzed ACTION: If technical holding times are exceeded, flag all positive results as estimated ("J") and sample quantitation limits as estimated ("UJ"), and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon reanalysis, reviewer must use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all results should be qualified "J", but the reviewer may determine that non-detect data are unusable ("R"). If holding times are exceeded by more than 28 days, all non detect data are unusable (R). 03O.1 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 24 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 3.0 Surrogate Recovery (Form II) 3.1 Are the BNA Surrogate Recovery Summaries (Form n) present for each of the following matrices: a. Low Water [__] __ __ b. Low Soil [__] __ __ c. MedSoil [__] __ __ 3.2 Are all the BNA Samples listed on the appropriate Surrogate Recovery Summaries for each of the following matrices: a. Low Water [__] __ b. Low Soil [__] __ c. Low Soil [__] __ ACTION; Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 3.3 Were outliers marked correctly with an asterisk? [__] __ 3.4 Were two or more base-neutral OR acid surrogate recoveries out of specification for any sample or method blank? [__] __ If yes, were samples reanalyzed? [__] __ Were method blanks reanalyzed? [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 25 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If all BNA surrogate recoveries are > 10% but two within the base-neutral or acid fraction do not meet SOW specifications, for the affe^d fraction only (i.e. base-neutral or acid compounds): 1. Flag all positive results as estimated ("J"). 2. Flag all non-detects as estimated detection limits (TIT) when recoveries are less than the lower acceptance limit 3. If recoveries are greater than the upper acceptance limit, do not qualify non-detects. If any base-neutral or acid surrogate has a recovery of < 10%: 1. Positive results for the fraction with < 10% surrogate recovery are qualified with "J". 2. Non-detects for that fraction should be qualified as unusable (R). 3.5 Are there any transcription/calculation errors between raw data and Form n? __ [__] __ ACTION; If large errors exist, call lab for explanation/resubmittal, make any necessary corrections and document effect in data assessments. 4.0 Matrix Spikes (Form III) 4.1 Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form HI) present? [__] __ __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 26 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 4.2 Were matrix spikes analyzed at the required frequently for each of the following matrices: a. Low Water [__] b. Low Soil [__] __ c. MedSoil [__] __ ACTION; If any matrix spike data are missing, take the action specified in 32 above. 4.3 How may BNA spike recoveries are outside QC limits? Water Soils ___ out of 22 ___ out of 22 4.4 How may RPD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? Water Soils ___ out of 11 ___ out of 11 ACTION: No action is taken on MS/MSD data alone. However, using informed professional judgement, the data reviewer may use the matrix spike and matrix spike duplicate results in conjunction with other QC criteria and determine the need for some qualification of the data. 5.0 Blanks (Form TV) 5.1 Is the Method Blank Summary (Form IV) present? [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 27 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 5.2 Frequency of Analysis: Has a reagent/method blank analysis been reported per 20 samples of similar matrix, or concentration level, and for each extraction batch? [__] __ __ 5.3 Has a BNA method blank been analyzed for each GC/MS system used? [__] __ __ (See SOW p. D - 59/SV, Section 8.7) ACTION; If any method blank data are missing, call lab for explanation/resubmittal. If not available, use professional judgement to determine if the associated sample data should be qualified. 5.4 Chromatography: review the blank raw data - chromatograms (RICs), quant reports or data system printouts and spectra. Is the chromatographic performance (baseline stability) for each instrument acceptable for BNAs? [__] __ __ ACTION! Use professional judgement to determine the effect on the data. 6.0 Contamination NOTE; "Water blank", "drill blanks" and "distilled water blanks" are validated like any other sample and are not used to quality the data. Do no confuse them with the other QC blanks discussed below. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 28 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 6.1 Do any method/instrument/reagent blanks have positive results (TCL and/or TIC) for BNAs? When applied as described below, the contaminant concentration in these blanks are multiplied by the sample dilution factor and corrected for % moisture where necessary. __ [__] 6.2 Do any field/rinse/blanks have positive BNA results (TCL and/or TIC)? __ [__] ACTION: Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet). NOTE; All field blank results associated to a particular group of samples (may exceed one per case) must be used to qualify data. Blanks may not be qualified because of contamination in another blank. Field Blanks must be qualified for surrogate, spectral, instrument performance or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. If gross contamination exists, all data in the associated samples should be qualified as unusable (R). STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 29 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 Sample cone > CRQL but < IQx blank Sample cone CRQL is < lOx blank value value & > lOx blank Common Phthalate Esters Flag sample result with a "U" Report CRQL & qualify "U" No qualification is needed Sample cone > CRQL but < 5x blank Sample cone < CRQL & is < 5x blank value Sample cone > CRQL value & >5 blank value Other Contaminants Flag sample result with a "U" Report CRQL & qualify "U" No qualification is needed. 6.3 YES NO N/A NOTE: Analytes qualified "U" for blank contamination are still considered as "hits" when qualifying for calibration criteria. ACTION; For TIC compounds, if the concentration in the sample is less than five times the concentration in the most contaminated associated blank, flag the sample data "R" (unusable). Are there field/rinse/equipment blanks associated with every sample? I__1 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 30 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: For low level samples, note in data assessment that there is no associated field/rinse/equipment blank. Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 GC/MS Instrument Performance Check 7.1 Are the GC/MS Instrument Performance Check Forms (Form V) present for Decafluorotriphenylphosphine (DFTPP)? [__] 7.2 Are the enhanced bar graph spectrum and mass/charge (m/z) listing for the DFTPP provided for each twelve hour shift? , [__] 7.3 Has an instrument performance check solution been analyzed for every twelve hours of sample analysis per instrument? [__] __ ACTION: List date, time, instrument ID, and sample analyses for which no associated GC/MS tuning data are available. DATE TIME INSTRUMENT SAMPLE NUMBERS ACTION; If lab cannot provide missing data, reject ("R") all data generated outside an acceptable twelve hour calibration interval. STANDARD OPERATING PROCEDURE Title: CLP Organic* Data Review Page 31 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If mass assignment is in error, flag all associated sample data as unusable (R). ACTION: If mass assignment is in error, flag all associated sample data as unusable (R). 7.4 Have the ion abundance been normalized to m/z 198? 7.5 Have the ion abundance criteria been met for each instrument used? ACTION: List all data which do not meet ion abundance criteria (attach a separate sheet). 7.6 Are there any transcription/calculation errors between mass lists and Form Vs? 7.7 Have the appropriate number of significant figures (two) been reported? ACTION: If large errors exist, call lab for explanation/resubmittal, make necessary corrections and document effect in data assessments. 7.8 Are the spectra of the mass calibration compound acceptable? ACTION! Use professional judgement to determine whether associated data should be accepted, qualified, or rejected. [__] __ __ [__1 [__] __ [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 32 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 8.0 Target Compound List (TCP Analvtes 8.1 Are the Organic Analysis Data Sheets (Form I BNA) present with required header information on each page, for each of the following: a. Samples and/or fractions as appropriate [__] __ __ b. Matrix spikes and matrix spike duplicates [__] __ __ c. Blanks [__] __ __ 8.2 Has GPC cleanup been performed on all soil/ sediment sample extracts? [__] __ __ ACTION: If data suggests that GPC was not performed, use professional judgement. Make note in "Contract Problems/Non-Compliance". 8.3 Are the BNA Reconstructed Ion Chromatograms, the mass spectra for the identified compounds, and the data system printouts (Quant Reports) included in the sample package for each of the following? a. Samples and/or fractions as appropriate [__] __ __ b. Matrix spikes and matrix spike duplicates [__] __ (Mass spectra not required) c. Blanks [__] __ ACTION; If any data are missing, take action specified in 3.2 above. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 33 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 8.4 Are the response factors shown in the Quant Report? [__] __ __ 8.5 Is chromatographic performance acceptable with respect to: Baseline stability? [__] __ __ Resolution? [__] __ __ Peak shape? [__] __ __ Full-scale graph (attenuation)? [__] __ __ Other:_________.________ [__] __ __ ACTION: Use professional judgement to determine the acceptability of the data. 8.6 Are the lab-generated standard mass spectra of identified BNA compounds present for each sample? [__] __ __ ACTION; If any mass spectra are missing, take action specified in 3.2 above. If lab does not generate their own standard spectra, make note in "Contract Problems/ Non-compliance". If spectra are missing, reject all positive data. 8.7 Is the RRT of each reported compound within 0.06 RRT units of the standard RRT in the continuing calibration? [__] __ 8.8 Are all ions present in the standard mass spectrum at a relative intensity greater than 10% also present in the sample mass spectrum? [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 34 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 8.9 Do sample and standard relative ion intensities agree within 20%? [__] __ ACTION; Use professional judgement to determine acceptability of data, if it is determined that incorrect identifications were made, all such data should be rejected (R), flagged "N" (Presumptive evidence of the presence of the compound) or changed to not detected (U) at the calculated detection limit. In order to be positively identified, the data must comply with the criteria listed in 8.7, 8.8, and 8.9. ACTION; When sample carry-over is a possibility, professional judgement should be used to determine if instrument cross-contamination has affected any positive compound identification. 9.0 Tentatively Identified Compounds (TIC) 9.1 Are all Tentatively Identified Compound Forms (Form I, Part B) present; and do listed TICs include scan number or retention time, estimated concentration and "JN" qualifier? [__] .,_ 9.2 Are the mass spectra for the tentatively identified compounds and associated "best match" spectra included in the sample package for each of the following: a. Samples and/or fractions as appropriate [__] __ b. Blanks [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 35 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If any TIC data are missing take action specified in 32 above. ACTION; Add "JN" qualifier if missing. 93 Are any TCL compounds (from any fraction) listed as TIC compounds (example: 1,2-dimethylbenzene is xylene a VOA TCL - and should not be reported as a TIC)? __ [__] ACTION; Flag with "R" any TCL compound listed as a TIC. 9.4 Are all ions present in the reference mass spectrum with a relative intensity greater than 10% also present in the sample mass spectrum? [__] __ 9.5 Do TIC and "best match" standard relative ion intensities agree within 20%? [__] __ ACTION; Use professional judgement to determine acceptability of TIC identifications. If it is determined that an incorrect identification was made, change identification to "unknown" or to some less specific identification (example: "C3 substituted benzene") as appropriate. Also, when a compound is not found in any blank, but is a suspected artifact of a common laboratory contaminant, the result should be qualified as unusable (R). 10.0 Compound Ouantitation and Reported Detection Limits 10.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Verify that the correct internal standard, quantitation ion, STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 36 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A and RRF were used to calculate Form I result Were any errors found? __ [__] __ 10.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, sample moisture? [__] __ ACTION: If errors are large, call lab for explanation/ resubmittal, make any necessary corrections and document effect in data assessments. ACTION; When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of the higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" and it's associated value on the original Form I and substituting the data from the analysis of the diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all From I's that should not be used, including any in the summary package. 11.0 Standard Data (GC/MS) 11.1 Are the Reconstructed Ion Chromatograms, and data system printouts (Quant Reports) present for initial and continuing calibration? [__] __ ACTION; If any calibration standard data are missing, take action specified in 3.2 above. 12.0 GC/MS Initial Calibration (form VI) 12.1 Are the Initial Calibration Forms (Form VI) present and complete for the BNA fraction? [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 37 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: If any calibration standard forms are missing, take action specified in 3.2 above. 12.2 Are response factors stable for BNAs over the concentration range of the calibration? (% Relative standard deviation (%RSD) < 30.0%) ACTION: Circle all outliers in red. NOTE: Although 20 BNA compounds have a minimum RRF and no maximum %RSD, the technical criteria are the same for all analytes. ACTION: If the % RSD is > 30.QS, qualify positive results for that analyte "J" and non-detects using professional judgement. When RSD > 90%, flag all non-detect results for that analyte R (unusable). NOTE; Analytes previously qualified "U" due to blank contamination are still considered as "hits" when qualifying for calibration criteria. 12.3 Are all BNA compound RRFs > 0.05? ACTION; Circle all outliers in red. ACTION: If any RRF < 0.05 1. "R" all non-detects. 2. "J" all positive results. [__1 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 38 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 12.4 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % RSD? (Check at least two values but if errors are found, check more.) __ [__] __ ACTION; Circle errors in red. ACTION: If errors are large, call lab for explanation/resubmittal, make any necessary corrections and note errors in data assessments. 13.0 GC/MS Continuing Calibration (Form Vin 13.1 Are the Continuing Calibration Forms (Form VII) present and complete for the BNA fraction? [__] __ 13.2 Has a continuing calibration standard been analyzed for every twelve hours of sample analysis per instrument? [__] ACTION; List below all sample analyses that were not within twelve hours of a continuing calibration analysis for each instrument used. ACTION: If any forms are missing or no continuing calibration standard has been analyzed within twelve hours of every sample analysis, call lab for explanation/resubmittal. If continuing calibration data are not available, flag all associated sample data as unusable ("R"). CUT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 39 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 13.3 Do any semivolatile compounds have a % Difference (%D) between the initial and continuing RRF which exceeds + 25.0% criteria? __ [__] __ ACTION: Circle all outliers in red. ACTION; Qualify both positive results and non-detects for the outlier compound(s) as estimated (J). When %D is above 90%, reject all non-detects for that analyte (R) unusable. 13.4 Do any semivolatile compounds have a RRF <0.05? __ [__] __ ACTION; Circle all oiitliers in red. ACTION; If RRF <0.05, qualify as unusable (R) associated non-detects and "J" associated positive values. 13.5 Are there any transcription/calculation errors in the reporting of average response factors (RRF) or % difference (%D) between initial and continuing RRFs? (Check at least two values but if errors are found, check more). __ [__] __ ACTION; Circle errors in red. ACTION: If errors are large, call lab fore explanation/resubmittal, make any necessary corrections and document effect in data assessments. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 40 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 14.0 Internal Standards (Form Vim 14.1 Are the internal standard areas (Form Vm) of every sample and blank within the upper and lower limits (-50% to + 100%) for each continuing calibration? [__] __ ACTION! List all the outliers below. Sample # Internal Std Area Lower Limit Upper limit (Attach additional sheets if necessary). ACTION: 1. If the internal standard area count is outside the upper or lower limit, flag with "J" all positive results and non-detects (U values) quantitated with this internal standard. 2. Non-detects associated with IS areas > 100% should not be qualified. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 41 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 3. If the IS area is below the lower limit (. 14.2 Are the retention times of the internal standards within 30 seconds of the associated calibration standard? [__] ACTION; Professional judgement should be used to qualify data if the retention times differ by more than 30 seconds. Duplicates 15.1 Were any field duplicates submitted for BNA analysis? [__] ACTION; Compare the reported results for field duplicates and calculate the relative percent difference. ACTION; Any gross variation between field duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 42 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A PART C; PESTICIDE/PCS ANALYSIS 1.0 Traffic Reports and Laboratory Narrative 1.1 Are Traffic Report Forms present for all samples? [__] __ __ ACTION: If no, contract lab for replacement of missing or illegible copies. 1.2 Do the Traffic Reports or SDG Narrative indicate any problems with sample receipt, condition of the samples, analytical problems or special circumstances affecting the quality of the data? [__] __ ACTION; If any sample analyzed as a soil, other then TCLP, contains 50%-90% water, all data should be qualified as estimated (J). If a soil sample, other than TCLP, contains more than 90% water, all data should be qualified as unusable (R). ACTION; If samples were not iced upon receipt at the laboratory, flag all positive results "J" and non-detects "UJ". 2.0 Holding Times 2.1 Have any PEST/PCB technical holding times, determined from date of collection to date of extraction, been exceeded? [__] __ Water and soil samples for PESTS/PCB analysis must be extracted within 7 days of the date of collection. Extracts must be analyzed within 40 days of the date extraction. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 43 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If technical holding times are exceeded, flag all positive results as estimated (J) and sample quantitation limits (UJ) and document in the narrative that holding times were exceeded. If analyses were done more than 14 days beyond holding time, either on the first analysis or upon re-analysis, the reviewer must use professional judgement to determine the reliability of the data and the effects of additional storage on the sample results. At a minimum, all the data should at least be qualified "J", but the reviewer may determine that non-detects are unusable (R). 3.0 Surrogate Recovery (Form II) 3.1 Are the PEST/PCB Surrogate Recovery Summaries (Form II) present for each of the following matrices? a. Low Water [__] b. Soil [__] 3.2 Are all the PEST/PCB samples listed on the appropriate Surrogate Recovery Summary for each of the following matrices? a. Low Water [__] b. Soil [__] ACTION: Call lab for explanation/resubmittals. If missing deliverables are unavailable, document effect in data assessments. 'TUT STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 44 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 3.3 Were outliers marked correctly with an asterisk? ACTION; Circle all outliers in red. 3.4 Were surrogate recoveries of TCX or DCB outside of the contract specification for any sample or blank? (60-150%) __ [__] ACTION; No qualification is done if surrogates are diluted out If recovery for both surrogates is below the contract limit, but above 10%, flag all results for that sample T. If recovery is < 10% for either surrogate, qualify positive results T and flag non-detects "R". If recovery is above the contract advisory limits for both surrogates qualify positive values "J". [__] 3.5 Were surrogate retention times (RT) within the windows established during the initial 3-point analysis of individual Standard Mixture A? [__] ACTION; If the RT limits are not met, the analysis may be qualified unusable (R) for that sample on the basis of professional judgement. 3.6 Are there any transcription/calculation errors between raw data and Form n? __ [__] ACTION; If large errors exist, call lab for explanation/resubmittal. Make any necessary corrections and document effect in data assessments. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 45 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 4.0 4.1 4.2 4.3 4.4 YES NO N/A Matrix Spikes (Form Tin Is the Matrix Spike/Matrix Spike Duplicate Recovery Form (Form ID) present? Were matrix spikes analyzed at the required frequency for each of the following matrices? (1 MS/MSD must be performed for every 20 samples of similar matrix or concentration level) a. Low Water b. Soil ACTION: If any matrix spike data are missing, take the action specified in 32 above. How may PEST/PCB spike recoveries are outside QC limits? [__] __ I__1 __ Water out of 12 Soil out of 12 How may RPD's for matrix spike and matrix spike duplicate recoveries are outside QC limits? Water out of 6 Soil _ out of 6 STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 46 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; No action is taken on MS/MSD data alone. However, using informed professional judgement, the data reviewer may use the matrix spike and matrix spike duplicate results in conjunction with other QC criteria and determine the need for some qualification of the data. 5.0 Blanks (Form IV) 5.1 Is the Method Blank Summary (Form IV) present? [__] 5.2 Frequency of Analysis: For the analysis of Pesticide/PCB TCL compounds, has a reagent/ method blank been analyzed for each SDG or every 20 samples of similar matrix or concentration or each extraction batch, whichever is more frequent? [__] ACTION; If any blank data are missing, take the action specified above in 32. If blank data is not available, reject (R) all associated positive data. However, using professional judgement, the data reviewer may substitute field blank data for missing method blank data. 5.3 Has a PEST/PCB instrument blank been analyzed at the beginning of every 12 hr. period following the initial calibration sequence? (minimum contract requirement). STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 47 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If any blank data are missing, call lab for explanation/resubmittals. If missing deliverables are unavailable, document the effect in data assessments. 5.4 Chromatography: Review the blank raw data - chromatograms, quant reports or data system printouts. Is the chromatographic performance (baseline stability) for each instrument acceptable for PEST/PCBs? [__] __ ACTION; Use professional judgement to determine the effect on the data. 6.0 Contamination NOTE; "Water blanks", "distilled water blanks" and "drilling water blanks" are validated like any other sample and are not used to qualify the data. Do not confuse them with the other QC blanks discussed below. 6.1 Do any method/instrument/reagent/cleanup blanks have positive results for PEST/PCBs? When applied as described below, the contaminant concentration in these blanks are multiplied by the sample Dilution Factor and corrected for % moisture when necessary. __ [__] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 48 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 6.2 Do any field/rinse blanks have positive PEST/PCB results? __ [__] ACTION; Prepare a list of the samples associated with each of the contaminated blanks. (Attach a separate sheet) NOTE; All field blank results associated to a particular group of samples (may exceed one per case or one per day) may be used to qualify data. Blanks may not be qualified because of contamination in another blank. Field blanks must be qualified for surrogate, or calibration QC problems. ACTION: Follow the directions in the table below to qualify TCL results due to contamination. Use the largest value from all the associated blanks. Sample cone > CRQL Sample cone < CRQL & Sample cone > CRQL but < 5 x blank is < 5x blank value & > 5 x blank value Flag sample result Report CRQL & No qualification with a "U"; qualify "U" is needed NOTE; If gross blank contamination exists, all data in the associated samples should be qualified as unusable (R). 6.3 Are there field/rinse/equipment blanks associated with every sample? [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 49 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; For low level samples, note in data assessment that there is no associated field/rinse/equipment blank. Exception: samples taken from a drinking water tap do not have associated field blanks. 7.0 Calibration and GC Performance 7.1 Are the following Gas Chromatograms and Data Systems Printouts for both columns present for all samples, blanks, MS/MSD? a. peak resolution check [__] __ __ b. performance evaluation mixtures [__] __ __ c. aroclor 1016/1260 [__] __ __ d. aroclors 1221, 1232, 1242, 1248, 1254 [__] __ __ e. toxaphene [__] __ __ f. low points individual mixtures A & B [__] __ __ g. med points individual mixtures A & B [__] __ __ h. high points individual mixtures A & B [__] .,_ __ i. instrument blanks [_] __ __ ACTION: If no, take action specified in 32 above. 7.2 Are Forms VI - PEST 1-4 present and complete for each column and each analytical sequence? [_] __ __ 7.3 Are there any transcription/calculation errors between raw data and Forms VI? _ [__] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 50 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION! If large errors exist, call lab for explanation/ resubmittal, make necessary corrections and document effect in data assessments. 7.4 Do all standard retention times, including each pesticide in each level of Individual Mixtures A & B, fall within the windows established during the initial calibration analytical sequence? (For Initial Calibration Standards, Form VI - PEST - 1). [_] ACTION: If no, all samples in the entire analytical sequence are potentially affected. Check to see if the chromatograms contain peaks within an expanded window surrounding the expected retention times. If no peaks are found and the surrogates are visible, non-detects are valid. If peaks are present and cannot be identified through pattern recognition or using a revised RT window, qualify all positive results and non-detects as unusable (R). For aroclors, RT may be outside the RT window, but the aroclor may still be identified from the individual pattern. 7.5 Are the linearity criteria for the initial analyses of Individual Standards A & B within limits for both columns? (%RSD must be < 20.0% for all analytes except for the 2 surrogates, which must not exceed 30.0 % RSD). See Form VI PEST - 2. [_] ACTION; If no, qualify all associated positive results generated during the entire analytical sequence "J" and all non-detects "UJ". When RSD >90% flag all non- detect results for that analyte R (unusable). STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 51 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 7.6 Is the resolution between any two adjacent peaks in the Resolution Check Mixture > 60.0% for both columns? (Form VI-PEST-4). [_] __ ACTION; If no, positive results for compounds that were not adequately resolved should be qualified "J". Use professional judgement to determine if non-detects which elute in areas affected by co-eluting peaks should be qualified "N" as presumptive evidence of presence or unusable (R). 7.7 Is Form VII - Pest-1 present and complete for each Performance Evaluation Mixture analyzed during the analytical sequence for. both columns? [_] __ ACTION; If no, take action as specified in 3.2 above. 7.8 Has the individual % breakdown exceeded 20.0% on either column. _ [__] - for 4,4' - DOT? _ [__] - for endrin? _ [__] Has the combined % breakdown for 4,4' - DDT/ Endrin exceeded 30.0% on either column? _ [__] (required in all instances) STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 52 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: 1. If any % breakdown has failed the QC criteria in either PEM in steps 2 and 17 in the initial calibration sequence (p. D-38/Pest SOW 3/90), qualify all sample analyses in the entire analytical sequence as described below. 2. If any % breakdown has failed the QC criteria in a PEM Verification calibration, review data beginning with the samples which followed the last in-control standard until the next acceptable PEM & qualify the data as described below. a. 4,4' - DDT Breakdown: If 4,4' - DOT breakdown is greater than 20.%: i. Qualify all positive results for DDT with "J". If DDT was not detected, but DDD and DDE are positive, then qualify the quantitation limit for DDT as unusable (R). ii. Qualify positive results for DDD and/or DDE as presumptively present at an approximated quantity (NJ). b. Endrin Breakdown: If endrin breakdown is greater than 20.0%: STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 53 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A i. Qualify all positive results for endrin with T. If endrin was not detected, but endrin aldehyde and endrin ketone are positive, then qualify the quantitation limit for endrin as unusable (R). ii. Qualify positive results for endrin ketone and endrin aldehyde as presumptively present at an approximated quantity (NJ). c. Combined Breakdown: If the combined 4,4' - DDT and endrin breakdown is greater then 30.0%. i. Qualify all positive results for DDT and endrin with "J". If endrin was not detected, but positive aldehyde and endrin ketone are positive, then qualify the quantitation limit for endrin as unusable (R). If DDT was not detected, but DDD and DDE are positive, then qualify the quantitation limit for DDT as unusable (R). ii. Qualify positive results for endrin ketone and endrin aldehyde as presumptively present at an approximated quantity (NJ). Qualify positive results for DDD and/or DDE as presumptively present at an approximated quantity (NJ). 7.9 Are the relative percent difference (RPD) values for all PEM analytes <25.0% (Form VH-PEST-1) [_] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 54 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION! If no, qualify all associated positive results generated during the analytical sequence "J" and sample quantitation limits "UJ". NOTE: If the failing PEM is part of the initial calibration. All samples are potentially affected. If the offending standard is a verification calibration, the associated samples are those which followed the last in-control standard until the next passing standard. 7.10 Have all samples been injected within a 12 hour period beginning with the injection of an instrument Blank? [_] __ 7.11 Is Form Vn - Pest-2 present and complete for INDA and INDB Verification Calibration analyzed? [_] __ 7.12 Are there any transcription/calculation errors between raw data and Form Vn - Pest - 2? _ [__] ACTION! If large errors exists, call lab for explanation/resubmittal, make any necessary corrections and document effect in data assessments. Under "Conclusions". 7.13 Do all standard retention times for each INDA and INDB Verification Calibration fall within the windows established by the initial calibration sequence? [_] __ STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 55 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A 7.14 Are RPD values for all verification calibration standard compounds < 25.0%? [_] __ __ ACTION: If the RPD is >25.0% for the compound being quantitated, qualify all associated positive results T and non-detects "UJ". The "associated samples" are those which followed the last in-control standard up to the next passing standard containing the analyte which failed the criteria. If the RPD is >90%, flag all non-detects for that analyte R (unusable). 8.0 Analytical Sequence Check (Form VIII-PEST) 8.1 Is Form VIII present and complete for each column and each period of analyses? [_] __ __ ACTION: If no, take action specified in 3.2 above. 8.2 Was the proper analytical sequence followed for each initial calibration and subsequent analyses? (See CLP SOW p. D-39 & D-41/PEST) [_] __ ACTION; If no, use professional judgement to determine the severity of the effect on the data and qualify it accordingly. Generally, the effect is negligible unless the sequence was grossly altered or the calibration was also out of limits. 9.0 Cleanup Efficiency Verification (Form IX) 9.1 Is From DC - Pest-1 Pest-1 present and complete for each lot of Florisil Cartridges used? (Florisil Cleanup is required for all Pest/PCB extracts.) [_] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 56 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; If no, take action specified in 32 above. If data suggests that florisil cleanup was not performed, make note in "Contract Problems/Non- Compliance". 9.2 Are all samples listed on the Pesticide Florisil Cartridge Check Form? [_] 9.3 If GPC Cleanup was performed, (mandatory for all' soil sample extracts) is Form IX - Pest-2 present? ACTION; If no, take action specified in 3.2 above. ACTION; If GPC was not performed when required, make note in" Contract Problems/Non-Compliance" section of data assessment. 9.4 Are percent recoveries (% R) of the pesticide and surrogate compounds used to check the efficiency of the cleanup procedures within QC limits: 80-120% for florisil cartridge check? [_] __ 80-110% for GPC calibration? [_] __ Qualify only the analyte(s) which fail the recovery criteria as follows: ACTION; If a R are < 80%, qualify positive results "J" and quantitation limits "UJ". Non-detects should be qualified "R" if zero %R was obtained for pesticide compounds. Use professional judgement to qualify positive results if recoveries are greater than the upper limit. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 57 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A NOTE; Sample data should be evaluated for potential interferences if recovery 2,4,5-trichlorophenol was > 5% in the Florisil Cartridge Performance Check analysis. Make note in Contract Problems/Non- Compliance section of reviewer narrative. NOTE: The raw data of the GPC Calibration Check analysis is evaluated for pattern similarity with previously run Aroclor standards. 10.0 Pesticide/PCB Identification 10.1 Is Form X complete for every sample in which a pesticide or PCB was detected? [_] __ __ 10.2 Are there any transcription/calculation errors between raw data and Forms 6E, 6G, 7E, 7D, 8D, 9A, B, 10A. _ [__] __ ACTION: If large errors exist, call lab for explanation/resubmittal, make necessary corrections and not error under "Conclusions". 10.3 Are retention times (RT) of sample compounds within the established RT windows for both analyses? [_] __ __ Was GC/MS confirmation provided when required (when compound concentration is > 10 ug/ml in final extract)? [_] __ ACTION; Use professional judgement to qualify positive results which were not confirmed by GC/MS. Qualify as unusable (R) all positive results which were not confirmed by second STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 58 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A GC column analysis. Also qualify as unusable (R) all positive results not meeting RT window unless associated standard compounds are similarly biased. (See Functional Guidelines). The reviewer should use professional judgement to assign an appropriate quantitation limit 10.4 Is the percent difference (% D) calculated for the positive sample results on the two GC columns < 25.0%? [_] __ ACTION; If the reviewer finds neither column shows interference for the positive hits, the data should be fagged as follows: % Difference Qualifier 25-50 % J 50-90 % JN > 90% R NOTE; The lower of the two values is reported on Form I. If using professional judgement, the reviewer determines that the higher results was more acceptable, the reviewer should replace the value and indicate the reason for the change in the data assessment. 10.5 Check chromatograms for false negatives, especially the multiple peak compounds toxaphene and PCBs. Were there any false negatives? _ [__] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 59 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; Use professional judgement to decide if the compound should be reported. If the appropriate PCB standards were not analyzed, qualify the data unusable (R). 11.0 Compound Quantitation and Reported Detection Limits 11.1 Are there any transcription/calculation errors in Form I results? Check at least two positive values. Were any errors found? ' _ [__] __ NOTE; Single-peak pesticide results can be checked for rough agreement between quantitative results obtained on the two GC columns. The reviewer should use professional judgement to decide whether a much larger concentration obtained on one column versus the other indicates the presence of an interfering compound. If an interfering compound is indicated, the lower of the two values should be reported and qualified as presumptively present at an approximated quantity (NJ). This necessitates a determination of an estimated concentration on the confirmation column. The narrative should indicate that the presence of interferences has interfered with the evaluation of the second column confirmation. 11.2 Are the CRQLs adjusted to reflect sample dilutions and, for soils, % mositure? [_] __ __ ACTION; If errors are large, call lab for explanation/resubmittal, make any necessary corrections and document effect in data assessments. STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 60 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION; When a sample is analyzed at more than one dilution, the lowest CRQLs are used (unless a QC exceedance dictates the use of higher CRQL data from the diluted sample analysis). Replace concentrations that exceed the calibration range in the original analysis by crossing out the "E" value on the original Form I and substituting it with data from the analysis of diluted sample. Specify which Form I is to be used, then draw a red "X" across the entire page of all Form I's that should not be used, including any in the summary package. ACTION; Quantitation limits effected by large, off-scale peaks should be qualified as unusable (R). If the interference is on-scale, the reviewer can provide an approximated quantitation limit (UJ) for each affected compound. 12.0 Chromatogram Quality 12.1 Were baselines stable? 12.2 Were any electropositive displacement (negative peaks) or unusual peaks seen? ACTION: Address comments under System Performance of data assessment. 13.0 Field Duplicates 13.1 Were any field duplicates submitted for PEST/PCB analysis? _ [__] STANDARD OPERATING PROCEDURE Title: CLP Organics Data Review Page 61 of 61 and Preliminary Review Date: January 1992 Number HW-6 Revision: 8 YES NO N/A ACTION: Compare the reported results for field duplicates and calculate the relative percent difference. ACTION; Any gross variation between field duplicate results must be addressed in the reviewer narrative. However, if large differences exist, identification of field duplicates should be confirmed by contacting the sampler. *PR00801/organic.dta ATTACHMENT 1 SOP NO. HW-6 PAGE 1 OF 16 TOTAL REVIEW CLP DATA ASSESSMENT Functional Guidelines for Evaluating Organics Analysis CaseNos. 22277.22312.22352 SDGNo. NA TARnRATOKY Knsem-Fast SITE Tutu Wells DATA ASSESSMENT: The current functional guidelines (USEPA Revision June 1991) for evaluating organic data have been applied. All data are valid and acceptable except those analytes which have been qualified with a "J" (estimated), "U" (undetected), "R" (unusable), or "JN" (presumptive evidence for the presence of the material at an estimated value). All action is detailed on the attached sheets. Two facts should be noted by all data users. First, the "R" flag means that the associated value is unusable and rejected. In other words, due to significant quality control (QC) problems, the analysis is invalid and provides no information as to whether the compound is present or not. "R" values should not appear on data tables because they cannot be relied upon, even as a last resort. The second fact to keep in mind is that no compound concentration, even if it has passed all QC tests, is guaranteed to be accurate. Strict QC serves to increase confidence in data, but any value potentially contains some error. Reviewer's Signature: Verified by: ATTACHMENT 1 SOP NO. HW-6 PAGE 2 OF 16 1. HOLDING TIME The amount of an analyte in a sample can change with time due to chemical instability, degradation, volatilization, etc. If the specified holding time is exceeded, the data may not be valid. Those analytes detected in the samples whose holding time has been exceeded are qualified as estimated (J). The non-detects (sample quantitation limits) are qualified as estimated (J), unless the holding times are grossly exceeded (over one week beyond maximum holding time), in which case the associated data are unusable and rejected (R). The following action was taken in the samples and analytes shown due to excessive holding time: All of the samples in the sixth quarterly sampling event at the Tutu Wells Site except Tillett were analyzed within the specified holding time as calculated from sample collection to volatile organic compound (VOC) analyses. Sample Tillett was reanalyzed with a dilution (DL), nineteen days outside the seven day holding time for unpreserved samples to quantitate total 1,2-dichloroethene (1,2-DCE). Therefore, the result for total 1,2-DCE from the DL analysis of sample Tillett is qualified as estimated (J). A holding time non-compliance summary for all samples is provided in A-l. 2. BLANK CONTAMINATION Quality assurance (QA) blanks, i.e., method, trip, field, rinse, and water blanks are prepared to identify any contamination that may have been introduced into the samples during sample preparation or field activity. Method blanks measure laboratory contamination. Trip blanks measure cross-contamination of samples during shipment. Field blanks measure cross- contamination of samples during field operations. If the concentration of the analyte is less than five times the blank contaminant level (ten times for the common contaminants), the analytes are negated and qualified as undetected, "U." The following analytes in the samples shown were qualified with "U" for these reasons: 0341 ATTACHMENT 1 SOP NO. HW-6 PAGE 3 OF 16 A) Method Blank Contamination All of the method blanks associated with the VOC analyses were reviewed to determine laboratory contamination levels. The method blanks are referred to by their file identification numbers for ease of correlation of the blank with the associated samples. The method blank (A2201) is reported to contain 0.45 micrograms per liter (ug/L) of methylene chloride, a common laboratory VOC contaminant. Samples Steele and Eglin I are associated with this blank. Methylene chloride was detected in both the samples at concentrations below the contract required quantitation limit (CRQL) and less than ten times (< lOx) the amount detected in the method blank. Therefore, the methylene chloride data for these samples are negated, raised to the CRQL, and qualified (U). The method blank (A2250) is reported to contain 0.15 ug/L of methylene chloride. Samples Harvey, Eglin III, Smith, and LaPlace are associated with this blank. Methylene chloride was detected in sample LaPlace at a concentration below the CRQL and < 1 Ox the amount detected in the method blank. Therefore, the methylene chloride data for sample LaPlace is negated, raised to the CRQL, and qualified (U). Methylene chloride was not detected in the remaining samples and therefore, no qualification of data is required. The method blank (A2314) is reported to contain 0.48 ug/L of methylene chloride. The DL analysis of the field replicate (FR) of sample Smith is associated with this blank. Methylene chloride was not quantitated using the DL and therefore, no qualification of data is required. The method blank (A2283) is reported to contain 0.22 ug/L of methylene chloride. Samples Tillett and trip blank (5/29/92) are associated with this blank. Methylene chloride was detected in both the samples at concentrations < lOx the amount detected in the method blank. Therefore, the methylene chloride data for these samples are negated and qualified (U). The methylene chloride result in sample Tillett is below the CRQL and therefore, the negated result is raised to the CRQL and reported with a (U). ATTACHMENT 1 SOP NO. HW-6 PAGE 4 OF 16 The method blank (A2822) is reported to contain 0.19 ug/L of methylene chloride. The DL and reanalysis of sample Tillett is associated with this blank. Methylene chloride was not quantitated using the dilution and therefore no qualification of data is required. Method blank (A2212) is free of contamination. B) Equipment Blank Contamination The equipment blank is a sample of deionized (DI) water passed through the decontaminated sampling equipment. It is used to identify any contaminant that may still be present in the sampling equipment and therefore may result in subsequent sample contamination. For the sixth quarter Tutu Well Site Sampling effort, well Gassett was sampled using a bailer. The remainder of the wells did not require any sampling equipment as all of the other wells had pumps installed. Therefore, the equipment blank collected is associated only with sample Gassett and is used to qualify this sample only. The equipment blank (5/27/92) is reported to contain 12 ug/L of methylene chloride. Methylene chloride is detected in sample Gassett at a concentration below the CRQL and < lOx the amount detected in the blank. Therefore, this result is negated, raised to the CRQL, and qualified (U). In addition, one tentatively identified compound (TIC) was also detected in the equipment blank. It is tentatively identified and estimated to be 4 ug/L of hexane (Retention time [RT] equal to [=] 6.54 minutes). Hexane is detected in sample Gassett at a concentration less than five times (< 5x) the amount detected in the blank; therefore the associated result is rejected and qualified (R) as unusable. ATTACHMENT 1 SOP NO. HW-6 PAGE 5 OF 16 C) Trip Blank Contamination The trip blank (5/27/92) is reported to contain 1 ug/L of methylene chloride. Samples Eglin I, Eglin II, Steele, and Gassett are associated with this blank. As previously discussed, the methylene chloride result for sample Gassett is negated based on the associated equipment blank which has a higher level of methylene chloride contamination. The methylene chloride data for samples Eglin I and Steele are negated based on the associated method blank results. Methylene chloride was detected in sample Eglin II at a concentration below the CRQL and < lOx the amount detected in the blank; therefore the result is negated, raised to the CRQL, and qualified (U). The trip blank (5/28/92) is reported to contain 0.46 ug/L of methylene chloride. Samples Harvey, Eglin m, Ramsay, Smith, Smith FR, and LaPlace are associated with this blank. Methylene chloride is detected in samples Ramsay and Smith FR at concentrations below the CRQL and < 1 Ox the amount detected in the blank. Therefore, the sample data are negated, raised to the CRQL, and qualified (U). As previously discussed, the methylene chloride result in sample LaPlace is negated based on the method blank contamination. Methylene chloride is not detected in samples Harvey, Eglin in, and Smith; therefore, no qualification of data is required. The trip blank (5/29/92) is reported to contain 1.1 ug/L of methylene chloride. Sample Tillett is associated with this blank. As previously discussed the methylene chloride result in the trip blank (5/29/92) is negated due to method blank contamination and therefore, no sample data are qualified based on the blank result. A summary of all contaminated blanks and associated samples is provided in Table A-2. 3. MASS SPECTROMETER TUNING Tuning and performance criteria are established to ensure adequate mass resolution, proper compound identification, and to some degree, sufficient instrument sensitivity. These criteria are not sample-specific. Instrument performance is determined using standard materials. TUT' ()O3 0344 ATTACHMENT 1 SOP NO. HW-6 PAGE 6 OF 16 Therefore, these criteria should be met in all circumstances. The tuning standard for VOCs is bromofluorobenzene (BFB). If the mass calibration is in error, all associated data will be classified as unusable, "R." . All mass calibrations associated with the VOC analyses in this project have met the QC criteria to ensure adequate mass resolution, proper compound identification and instrument response. 4. CALIBRATION Satisfactory instrument calibration is established to ensure that the instrument is capable of producing acceptable quantitative data. An initial calibration demonstrates that the instrument is capable of giving acceptable performance at the beginning of an analytical sequence. The continuing calibration checks document that the instrument is giving satisfactory daily performance. A) Response Factor The response factor (RF) measures the instrument's response to specific chemical compounds. The response factor for the Target Compound List (TCL) must be > 0.05 (a ratio of areas) in both the initial and continuing calibrations. A value < 0.05 indicates a serious detection and quantitation problem (poor sensitivity). For analytes detected in the sample for which the response factor is < 0.05, positive detects will be qualified as estimated, (J). All non-detects for that compound will be rejected (R). The initial continuing calibration verification (ICV) performed on 5/29/92 had a RF less than (<) 0.05 units for 2-hexanone (0.03216). All the samples in the project are associated with this ICV (Steele, Eglin I, Eglin II, Gassett, equipment blank (5/27/92), trip blank (5/27/92), Harvey, Eglin III, Ramsay, Smith, LaPlace, Smith FR, trip blank (5/28/92), Tillett, and trip blank (5/29/92)). 2-Hexanone was not detected in these samples; therefore the results are biased low and are rejected (R). 0343 ATTACHMENT 1 SOP NO. HW-6 PAGE 7 OF 16 The continuing calibration verifications (CCVs) performed on 5/29/92 (0.03597), 5/30/92 (0.03148), 6/01/92 (0.03134), 6/2/92 (0.02991), 6/4/92 (0.03092), and 6/25/92 (0.03734) have RFs <0.05 units for 2-hexanone (RFs are in parentheses). The 2-hexanone data in all samples are rejected based on the RF criteria associated with the ICV. No further qualifications are necessary based on the associated CCVs. In addition, the CCV performed on 5/29/92 has a RF < 0.05 units for acetone. Samples Steele and Eglin I are associated with this CCV. Acetone is not detected in these samples; therefore the associated data are biased low and are rejected (R). The CCV performed on 6/2/92 has a RF < 0.05 units for 4-methyl-2-pentanone. Samples Tillett and trip blank (5/29/92) are associated with this blank. 4-Methyl-2-pentanone is not detected in these samples; therefore, the associated data are biased low and are rejected (R). The dilution and reanalysis of samples Steele and Tillett are associated with CCVs which have RFs < 0.05 units for 2-hexanone. 2-Hexanone is not quantitated using the dilutions, and therefore, no qualification of data is required for these sample dilutions. 5. CALIBRATION (B) Percent Relative Standard Deviation and Percent Difference Percent relative standard deviation (%RSD) is calculated from the initial calibration and is used to indicate the stability of the specific compound response factor over increasing concentration. Percent difference (%D) compares the response factor of the continuing calibration check to the average response factor (RRF) from the initial calibration. Percent D is a measure of the instrument's daily performance. Under Revision 3.0 for Method 524.2 %RSD must be < 20% and %D must be <30%. A value outside of these limits indicates potential detection and quantitation errors. All positive results are flagged as estimated, "J," and non-detects are flagged "UJ" if %D is > 30% or %RSD > 20%. If there is a gross deviation (i.e., > 90%) of %RSD and %D, the non-detects may be rejected (R). ATTACHMENT 1 SOP NO. HW-6 PAGE 8 OF 16 The %RSDs in all of the ICVs associated with this project are within the QC limit; therefore, data qualification is unnecessary. The CCV performed on 5/30/92 has a %D for acetone (48.73%) outside the method specified limit (< 30%). Samples Steele DL, Gassett, Eglin n, trip blank (5/27/92), equipment blank (5/27/92), trip blank (5/28/92), Ramsay, and Smith FR are associated with this CCV. Acetone is not quantitated using the DL and reanalysis of sample Steele; the acetone data in the remaining samples are qualified as estimated (J). 6. SURROGATES All samples are spiked with surrogate compounds prior to sample preparation or analysis to evaluate overall laboratory performance and efficiency of the analytical technique. If the measured surrogate concentrations were outside contract specifications, qualifications were applied to the samples and analytes as shown below. Volatile surrogate percent recoveries (%Rs) for this project are within the corresponding QC limits (toluene-d8 [88-110%], bromofluorobenzene [86-115%], l,2-dichloroethane-d4 [76-114%]). %R data were transcribed correctly from the quantitation reports to the Form His. 7. INTERNAL STANDARDS PERFORMANCE Internal standard (IS) performance criteria ensure that the gas chromatograph/mass spectrophotometer (GC/MS) sensitivity and response are stable during every analytical run. The internal standard area count must not vary by more than a factor of two (-50% to +100%) from the associated continuing calibration standard. The retention time of the internal standard must not vary more than 30 seconds from the associated continuing calibration standard. If the area count is outside the (-50 % to +100%) range of the associated standard, all of the positive results for compounds quantitated using that IS are qualified as estimated (J); and all non-detects as estimated at the reporting limit (UJ), or unusable and rejected (R), if there is a severe loss of sensitivity. ATTACHMENT 1 SOP NO. HW-6 PAGE 9 OF 16 If an internal standard retention time varies by more than 30 seconds, the reviewer will use professional judgment to determine either partial or total rejection of the data for that sample fraction. All of the IS area counts and retention times are within above mentioned QC limits for the VOC analyses. Bromochloromethane, 1,4-difluorobenzene, and chlorobenzene were the three internal standards used to quantitate the data for this SDG. All retention times, area counts, and chromatography for the IS compounds are acceptable. 8. COMPOUND IDENTIFICATION A) Volatile and Semi-volatile Fractions TCL compounds are identified on the GC/MS by using the analyte's relative retention time (RRT) and by comparison to the ion spectra obtained from known standards. For the results to be a positive hit, the sample peak must be within +. 0.06 RRT units of the standard compound and have an ion spectra that has a ratio of the primary and secondary m/e intensities within 20% of that in the standard compound. For the TICs, the ion spectra must match accurately. In cases where there is not an adequate ion spectrum match, the laboratory may have provided false-positive identifications. TCL compound identification by GC/MS was based on comparison of the analyte RRT and ion spectra to those obtained from known standard spectra. Positive hits were reviewed for all samples and the following discrepancies were noted in meeting the RRT criteria of ±0.06. RRT criteria were exceeded in the VOC analyses for total 1,2-DCE. This discrepancy is attributed to the presence of geometric isomers. 1,2-DCE exists as cis and trans isomers, which are not entirely resolvable using Method 524.2, Revision 3.0. Since the relative intensity between the two isomer peaks varies, quantitation is based on the retention time of the peak with the higher intensity. As the ionic spectra for 1,2-DCE accurately matches the standard compound spectrum, no data have been qualified based on RRT deviations. ATTACHMENT 1 SOP NO. HW-6 PAGE 10 OF 16 TICs with positive identifications based on presumptive evidence of the detected compound as an estimated value are qualified "JN." All TIC data are qualified as estimated (J) since these compounds are not calibrated for. 9. MATRIX SPIKE/MATRIX SPIKE DUPLICATE The matrix spike/matrix spike duplicate (MS and MSD) data are generated to determine the long-term precision and accuracy of the analytical method in various matrices. The MS and the MSD may be used in conjunction with other QC criteria for some additional qualification of the data. The MS and MSD were performed on sample Eglin I to determine sample matrix interferences on the analytical results. The sample was spiked in duplicate at a level of 5 ug/L with the following analytes (QC limits for recovery are within parentheses): 1,1-dichloroethene (61-145%), trichloroethene (71-120%), benzene (76-127%), toluene (76-125%), and chlorobenzene (75-130%). All ten matrix spike %Rs meet specified QC criteria. Relative percent differences (RPDs) between matrix spike and matrix spike duplicate %Rs are within QC limits (11- 14%). Therefore, it appears that there is no matrix bias affecting the data. 10. OTHER QC DATA OUT OF SPECIFICATION A) Method Detection Limit Study The method detection limit (MDL) study associated with Method 524.2 was performed on July 29, 1991. The MDL determination was based on the analysis of seven replicates of reagent water fortified at a concentration of 1.0 ug/L (ketones at 5 ug/L, and 1,2-DCE at 2 ug/L) with the TCL analytes. The laboratory MDL was calculated as the product of the standard deviation of seven replicate analyses and the student's t value for the 99% confidence level with six degrees of freedom (/ = 3.143). ATTACHMENT 1 SOP NO. HW-6 PAGE 11 OF 16 Section 10.3.3 of Method 524.2 states that for every analyte and surrogate, the mean accuracy, expressed as a percentage of the true value, should be 80-120% and the %RSD < 20%. In the MDL study performed in support of the VOC analyses for the Tutu Wells site, the following analytes did not meet the accuracy criteria required prior to sample analyses: Analyte Mean Accuracy (%) Methylene chloride 137 2-Butanone 79 Dibromochloromethane 68 trans 1,3-Dichloropropane 70 Bromoform 56 The %RSDs for all analytes were within QC criteria (< 20%). None of the data is qualified based on the results from the MDL study. B) Laboratory Fortified Blanks As per the QC requirements in Method 524.2 (Revision 3.0) and the site SAMP, a laboratory fortified blank (LFB) containing each target analyte at a known concentration is to be analyzed with every batch of samples processed using the method. For the sixth quarter Tutu Wells Site sampling effort, LFBs were prepared at a concentration of 1 ug/L for all TCL analytes except ketones and 1,2-DCE. Ketones were analyzed at 5 ug/L and 1,2-DCE was analyzed at 2 ug/L. The 1,2-DCE matrix fortification was comprised of 1 ug/L of the cis isomer and 1 ug/L of the trans isomer injected together, and quantitated as total 1,2-DCE. The LFBs were used to evaluate the accuracy of the method and estimate whether MDLs were achieved for every associated analytical sequence. If the laboratory did not meet these QC criteria, the deficiencies had to be rectified prior to further sample analyses (as specified in Method 524.2, Section 10.3). QC criteria for data assessment were modified for the VOC analyses of the Tutu well samples. Based on USEPA guidance (dated December 4, 1990) regarding ATTACHMENT 1 SOP NO. HW-6 PAGE 12 OF 16 additional quality assurance/quality control (QA/QC) requirements when Method 524.2 is used for aqueous sample analysis, the 80-120% criteria for the accuracy assessment of LFB were expanded to 50-150%, for the ketones (acetone, 2-butanone, 4-methyl-2-pentanone, and 2-hexanone). Therefore, for this validation, associated data for all TCL analytes with LFB recoveries < 50% are rejected and qualified "R." For LFB analyte recoveries in the range of 50-79% for TCL analytes other than ketones, the associated sample data are qualified as estimated (J). For LFB analyte recoveries > 150%, associated sample data are not qualified. The LFBs associated with this project, which have analyte recoveries outside of the required QC guidelines, are summarized below. All LFBs are referred to by their file identification numbers as well as the dates they were analyzed. The LFB (A2203) analyzed on 5/29/92 has %Rs outside QC limits for the following compounds: Compound Recovery (%) Methylene chloride 148 Bromoform 74 Samples Steele and Eglin I are associated with this blank. Associated sample data for bromoform are estimated at the quantitation limit (UJ). The LFB (A2213) analyzed on 5/30/92 has %Rs outside QC limits for the following compounds: Compound Recovery (%) Methylene chloride 135 Bromoform 77 Samples Gassett, Eglin II, trip blank (5/27/92), equipment blank (5/27/92), trip blank (5/28/92), Ramsay, and Smith FR are associated with this blank. Associated sample data for bromoform are estimated at the quantitation limit (UJ). ATTACHMENT 1 SOP NO. HW-6 PAGE 13 OF 16 The LFB (A2251) analyzed on 6/1/92 has %Rs outside QC limits for the following compounds: Compound Recovery f%) Chloromethane 126 2-Butanone 74 Samples Harvey, Eglin III, Smith, and LaPlace are associated with this blank. Associated sample data for 2-butanone are estimated at the quantitation limit (UJ). The LFB (A2285) analyzed on 6/2/92 has %Rs outside QC limits for the following compounds: Compound Recovery (%) Chloromethane , 79 Methylene chloride 128 Carbon disulfide 75 Samples Tillett and trip blank 5/29/92 are associated with this blank. Associated sample data for Chloromethane and carbon disulfide are estimated at the quantitation limit (UJ). The LFB (A2823) analyzed on 6/25/92 has %Rs outside QC limits for the following compounds: Compound Recovery (%) Vinyl chloride 121 Benzene 125 1,2-Dichloropropane 125 Bromoform 78 Chloroethane 151 Sample Tillett DL is associated with this blank. Only one analyte, total 1,2-DCE is quantitated using the dilution performed on sample Tillett. Therefore, the associated data do not require qualification based on the exceedance in the %Rs in this LFB. ATTACHMENT 1 SOP NO. HW-6 PAGE 14 OF 16 C) Field Duplicate Field duplicate or replicate samples are taken and analyzed as an indication of overall precision. These analyses measure both field and laboratory precision; therefore, the results may have more variability than laboratory duplicates that measure only laboratory performance. Sample Wess (listed as such on the chain-of-custody record) is a field replicate of Smith, and in all discussions and tables in this report is referred to as Smith FR. The RPD between results in both samples is calculated only for positive detects greater than four times the method detection limit, and not for estimated or undetected results. The results reported for both samples Smith and Smith FR were compared and the RPD calculated for total 1,2-DCE, trichloroethene, and tetrachloroethene. The RPDs calculated are within the required limit (< 20%) and therefore, no qualification of data is required. 11. SYSTEM PERFORMANCE AND OVERALL ASSESSMENT It is appropriate for the data reviewer to make professional judgments and express concerns and comments on the validity of the overall data for a case. This is particularly appropriate when there are several QC criteria out of specification. The additive nature of QC factors out of specifications is difficult to assess in an objective manner. The reviewer has a responsibility to inform the person using the data concerning data quality and data limitations to assist the individual in avoiding inappropriate use of the data. Therefore, this review has presented all QC factors that may affect the quality of the data. Overall, the data submitted by Enseco-East are of good quality and acceptable completeness. Aside from the exceptions summarized below, the majority of the data for this project are valid and usable. Non-detect data for 2-hexanone in all the samples in this project are biased low and are rejected due to poor sensitivity, as determined from the consistently low instrument RFs. Some acetone and 4-methyl-2-pentanone data are also rejected due to poor sensitivity. ATTACHMENT 1 SOP NO. HW-6 PAGE 15 OF 16 Some acetone data are estimated due to unacceptable instrument performance on a daily basis. This is indicated by the %D in the associated continuing calibration verification standard being above the specified QC limit. The result for 1,2-DCE in sample Tillett quantitated using a dilution is estimated because the analysis was conducted outside the holding time. Much of the sample data for methylene chloride are negated since their presence is the result of blank contamination (laboratory, equipment, and trip). One tentatively identified compound in sample Gassett is negated, and subsequently rejected, since its presence is due to field blank contamination. Much of the sample data for bromoform, and some sample data for 2-butanone, carbon disulfide, and chloromethane are estimated due to poor recovery in the associated LFBs. All TICs in this SDG are qualified as "J", because the laboratory does not calibrate the GC/MS for these compounds. TICs that are "positively identified" are qualified "JN", indicating presumptive evidence of the detected compound at an estimated value. TCL analytes that required re-analysis upon dilution are qualified "D." The July 1991 MDL study resulted in some compounds not meeting the preliminary accuracy requirements needed to establish the baseline MDL for the low level analysis. The same compounds (bromoform and 2-butanone) that had poor recovery in the LFB analyses, had low recovery in the MDL accuracy measurement criteria. The precision requirement between replicate measurements in the MDL study (RSD < 20%) was met for all compounds. Methylene chloride had an elevated recovery that can be attributed to laboratory contamination. 12. CONTRACT PROBLEMS (NON-COMPLIANCE) For some samples, concentrations of 1,2-DCE and PCE were high, and the analytes could not be accurately quantitated within the specified calibration range. ATTACHMENT 1 SOP NO. HW-6 PAGE 16 OF 16 Therefore, dilutions of the sample were reanalyzed for these specific analytes. However, no supporting Form I(s) were provided for the dilutions. The laboratory fortified blanks did not meet all of the method criteria as required. In accordance with the method, all deficiencies should be located and remedied prior to sample analysis. The case narratives submitted by Enseco along with the data packages contained inaccuracies. 13. This package contains re-extraction, re-analysis or dilution. Upon reviewing the QA results, the following Form I(s) are identified to be used: Samples Steele, Harvey, Smith, Smith FR, LaPlace, and Tillett were analyzed at a dilution due to the presence of high concentrations of target analytes. All the dilution data appear on the initial Form I data sheets. PROOeOl-DV/tutjul Tin' Region II ORGANIC REGIONAL DATA ASSESSMENT —— CASE NO. 22277. 22312. 22352______ SITE Tutu Wells. St. Thomas. U.S. Virgin Islands LABORATORY Enseco-East________ NO. OF SAMPLES/ MATRIX_____ 15/Water________ _________________ REVIEWER (IF NOT ESD)JjJ/A_______ SOW# OLMQ1.0. March 1990 (including REVIEWER'S NAME Uma Parasar______ further revisions) DPO: ACTION____ FYIJ£________ COMPLETION DATE July 20. 1992_____ DATA ASSESSMENT SUMMARY VOA BNA PEST 1. HOLDING TIMES _Q___ N/A N/A 2. GC/MS TUNE/INSTR. PERFORM. _Q___ N/A N/A 3. CALIBRATIONS _M___ N/A N/A 4. BLANKS _Q___ N/A N/A 5. SYSTEM MONITORING COMPOUNDS _Q____ N/A N/A 6. MATRIX SPIKE/DUP _Q___ N/A N/A 7. OTHER QC _Q___ N/A N/A 8. INTERNAL STANDARDS _Q___ N/A N/A 9. COMPOUND IDENTIFICATION _Q___ N/A N/A 10. SYSTEM PERFORMANCE _Q___ N/A N/A 11. OVERALL ASSESSMENT _Q___ N/A N/A O = Data had no problems/or qualified due to minor problems. M = Data qualified due to major problems. Z = Data unacceptable. X = Problems, but do not affect data. ACTION ITEMS: Some data for common blank contaminants have been negated based on blank contamination. Some data have been estimated based on calibration criteria, laboratory fortified blank (LFB) recoveries, and analysis outside holding time. Some data for volatile organic analysis (VOA) have been rejected for response factors. AREAS OF CONCERN:__None___________________________________ NOTABLE PERFORMANCE: Overall data is valid and can be used with some exceptions. PR00801-DV3/071692.dta TUT ATTACHMENT NO. 2 TABLES GERAGHTY & MILLER. INC ( f Table A-1. Volatile Organic Analysis Holding Time Summary, Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Sample Identifier Eglin I Eglin II Steele Gassett Equipment Blank (5/27/92) Trip Blank (#27/92) Trip Blank (5/28/92) Harvey Eglin III Ramsay Smith LaPlace Smith FR Tillett Trip Blank (5/29/92) Tillett DL Matrix Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Aqueous Preserved Yes Yes No Yes Yes Yes Yes No Yes Yes No Yes No No Yes No Date Collected 27-May-92 27-May-92 27-May-92 27-May-92 27-May-92 27-May-92 28-May-92 28-May-92 28-May-92 28-May-92 28-May-92 28-May-92 28- May-92 29-May-92 29-May-92 29-May-92 Date Received 28-May-92 28-May-92 28-May-92 28-May-92 28-May-92 28-May-92 29-May-92 29- May-92 29-May-92 29-May-92 29-May-92 29-May-92 29-May-92 30-May-92 30-May-92 30-May-92 Date Analyzed 29-May-92 30-May-92 29- May-92 30-May-92 30-May-92 30-May-92 30-May-92 Ol-Jun-92 Ol-Jun-92 30-May-92 Ol-Jun-92 Ol-Jun-92 30-May-92 03-Jun-92 03-Jun-92 25-Jun-92 Days from Collection to Analysis 2 3 2 3 3 3 2 3 3 2 3 3 2 4 4 26 Days Holding Time Exceeded 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 19 I Field replicate. '„ Dilution. R0080Vtablea-l.wk3 GERAGHTY & MILLHR. INC Table A-2. Summary of Volatile Organic Compound Contaminated Blanks and Associated Ground-Water Samples, Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Blank Identifier (Date Sampled or File I.D.) Equipment Blank (5/27/92) Trip Blank (5/27/92) Method Blank (A2201) Trip Blank (5/28/92) Method Blank (A2250) Method Blank (A23 14) Trip Blank (5/29/92) Method Blank (A2283) Method Blank (A2822) I.D. Identification. DL Dilution. FR Field replicate. Date Analyzed 5/30/92 5/30/92 5/29/92 5/30/92 6/01/92 6/04/92 6/03/92 6/02/92 6/25/92 Associated Sample(s) Eglin I, Eglin II, Steele, Gassett Eglin I, Eglin II, Steele, Gassett Eglin I, Steele Harvey, Eglin III, Ramsay, Smith, LaPlace, Smith FR Harvey, Eglin III, Smith, LaPlace Smith FR DL Tillett Trip Blank (5/29/92), Tillett Tillett DL *PROOS01/uble»-2.wtJ T U T GERAGHTY & MILLER. INC. Table A-3. Summary of Laboratory Fortified Blanks with Exceeded QC Criteria and Associated Ground-Water Samples, Sixth Sampling Event, May 1992, Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Sample Identifier (File I.D.) Date Analyzed Associated Samples Compounds with Exceeded QC Criteria LFB (A2203) LFB (A2213) 5/29/92 5/30/92 Eglin I, Steele Eglin II, Gassett, Trip Blank (5/27/92), Equipment Blank (5/27/92), Trip Blank (5/28/92), Ramsay, Smith FR Methylene chloride (148%), Bromoform (74%) Methylene chloride (135%), Bromoform (77%) 1 1 - --31 J _ Ii 1 m LFB (A2251) 6/1/92 LFB (A2285) 6/2/92 LFB (A2823) 6/25/92 I.D. Identification. QC Quality control. LFB Laboratory fortified blank. FR Field replicate. DL Dilution. Harvey, Eglin III, Smith, Chloromethane (126%), LaPlace 2-Butanone (74%) Tillett, Chloromethane (79%) Trip Blank (5/29/92) Methylene chloride (128%), Carbon disulfide (75%) Tillett DL Vinyl chloride (121%), Benzene (125%), 1,2-Dichloropropane (125%), Bromoform (78%), Chloroethane (151%) *PR0080Vublea-3.wt3 GERAGHTY & MILLER. INC. TUT OO3 0360 Table A-4. Concentrations of Volatile Organic Compounds in Ground-Water Samples Collected in May 1992 Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Page 1 of 2 S«nple ID: Eglin I Eglin n Analyte Edte: 27-M«y-92 27-M«y-92 Chloromethane 0.5 U 0.5 V Bromomethane O.S U O.S U Vinyl chloride O.S U O.S U Chloroethane O.S U O.S U Methylene chloride O.S U O.S U Acetone R 2 UJ Carbon disulfide O.S U O.S U 1,1-Dichloroethene O.S U O.S U 1,1-Dichloroethane O.S U O.S U 1 ,2-Dichloroetheae (cis/trant) 13 31 Chloroform O.OS J 0.09 J 1,2-Dichloroethane O.S U O.S U 2-BuUuionc 2 U 2 U 1,1,1-Trichloroethane O.S U O.S U Carbon tetrachloride O.S U O.S U Bromodichloromethane O.S U O.S U 1 ,2-Dichloropropane O.S U O.S U trans-l,3-Dichloropropene O.S U O.S U Trichloroethene 6.3 14 Dibromochloromethane O.S U O.S U 1,1,2-Trichloroethane O.S U O.S U Benzene O.S U 0.07 J ci»-l,3-Dichloropropene O.S U O.S U Bromoform O.S UJ O.S UJ 4-Methyl-2-pentanone 2 U 2 U 2-Hexanone R R 1,1,2,2-Tetrachloroethane O.S U O.S U Tetrachloroethene 14 36 Toluene 0.06 J O.S U Chlorobenzene O.S U O.S U Ethylbenzene O.S U O.S U Styrene O.S U O.S U Xylenei (total) O.S U O.S U Eglin m 28-May-92 O.SU 0.5 U O.SU O.SU O.SU 2U O.SU O.SU O.SU 31 0.07 J O.SU 2UJ O.SU O.SU O.SU O.SU O.SU 14 O.SU O.SU O.SU O.SU O.SU 2U R O.SU 39 O.SU O.SU 0.5 U O.SU O.SU Analyte concentrations in microgrami iper liter (parts per billion [ppb]). Analyses were performed by Enseco-East of Somerset, New Jersey, using OtMett 27-M«y-92 O.SU O.SU O.SU O.SU O.SU 2UJ O.SU O.SU O.SU O.SU O.SU O.SU 2U O.SU O.SU O.SU O.SU O.SU 0.06 J O.SU O.SU O.SU O.SU 0.5 UJ 2U R O.SU O.SU O.SU O.SU O.SU O.SU O.SU Harvey 28-May-92 6.2 u 6.2 U 6.2 U 6.2 U 6.2 U 25U 6.2 U 6.2 U 6.2 U 41 6.2 U 6.2 U 25 UJ 6.2 U 6.2 U 6.2 U 6.2 U 6.2 U 29 6.2 U 6.2 U 6.2 U 6.2 U 6.2 U 25U R 6.2 U 350 6.2 U 6.2 U 6.2 U 6.2 U 6.2 U USEPA Method 524.2, U Place 28-M«y-92 2u 2U 2U 2U 2U 8U 2U 2U 2U 100 0.44 J 2U 8UJ 2U 2U 2U 2U 2U 19 2U 2U 2U 2U 2U 8U R 2U 60 2U 2U 2U 2U 2U Revision 3.0. lUmuy 28-Miy-92 O.SU O.SU O.SU O.SU O.SU 2UJ O.SU O.SU O.SU 9.5 1.3 O.SU 2U O.SU O.SU 0.44 J O.SU O.SU 2.4 O.SU O.SU O.SU O.SU 0.5 UJ 2U R O.SU 20 O.SU O.SU O.SU O.SU O.SU Smith 28-M«y-92 2.5 u 2.5 U 2.5 U 2.5 U 2.5 U 10 U 2.5 U 2.5 U 2.5 U 40 2.5 U 2.5 U 10 UJ 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U IS 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U 10 U R 2.5 U 140 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U Smith FR 28-May-92 O.SU O.SU O.SU O.SU O.SU 2UJ O.SU O.SU O.SU 37 0.2 J O.SU 2U O.SU O.SU O.SU O.SU O.SU 14 O.SU O.SU O.SU O.SU 0.5 UJ 2U R O.SU 150 D O.SU O.SU O.SU O.SU O.SU Steele 27-Mty-92 1.2 U 1.2 U 2 1.2 U 1.2 U R 1.2 U 1.2 U 1.2 U ISO D 1.2 U 1.2 U 5U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U 27 1.2 U 1.2 U 1.2 U 1.2 U 1.2UJ SU R 1.2 U 40 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U TiUett 29-M«y-92 2.5 uJ 2.5 U 3.2 2.5 U 2.5 U 10 U 2.5 UJ 2.5 U 2.5 U 470 DJ I.2J 2.5 U 10 U 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U 59 2.5 U 2.5 U 0.8 J 2.5 U 2.5 U R R 2.5 U 200 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U Equipment Blink 27-M*y-92 O.SU O.SU O.SU O.SU 12 2UJ O.SU O.SU O.SU O.SU O.SU O.SU 2U O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SUJ 2U R O.SU O.SU O.SU O.SU O.SU O.SU O.SU Trip Blank 27-May-92 O.SU O.SU O.SU O.SU 1 2UJ O.SU O.SU O.SU O.SU O.SU O.SU 2U O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SUJ 2U R O.SU O.SU O.SU O.SU O.SU O.SU O.SU D Analyte identified at a secondary dilution. J Result is detected below the reporting limit and/or is an estimated concentration. U Compound or element analyzed for, but not detected at the corresponding reporting limit, u Reporting limit raised due to high levels of target analytes. R Result rejected. FR Field replicate of previous sample. TUT GERAGHTY # MILI.I-R. INC Table A-4. Concentrations of Volatile Organic Compounds in Ground-Water Samples Collected in May 1992 Tutu Wells Site, St. Thomas, U.S. Virgin Islands. Page 2 of 2 Sample ID: Trip Blank Trip Blank Anilyte Date: 28-May-92 29-May-92 Chloromethane Bromomethane Vinyl chloride Chloroethane Metbylene chloride Acetone Carbon disulflde 1,1-Dichloroethene 1,1-Dichloroethane 1 ,2-Dkhloroethene (cUArans) Chloroform 1,2-Dkhloroethane 2-Butanone 1 , 1 , 1-Trkhloroethane Carbon tetrachloride Bromodichloromethane 1 ,2-Dichloropropane trans- 1 ,3-Dichloropropene Trichloroethene Dibroraochloromethane 1 , 1 ,2-Trichloroethane Benzene cis- 1 ,3-Dichloropropene Bromoform 4-Methyl-2-pentanone 2-Hexanone 1 , 1 ,2,2-Tetrachloroethane Tetracbloroethene Toluene Chlorobenzene Ethylbenzene Styrene Xylenes (total) 0.5 U 0.5 U O.SU 0.5 U 0.46 J 2UJ O.SU O.SU O.SU O.SU O.SU O.SU 2U O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SUJ 2U R O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SUJ O.SU O.SU O.SU 1.1U 2U O.SUJ O.SU O.SU O.SU O.SU O.SU 2U O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU O.SU R R O.SU O.SU O.SU O.SU O.SU O.SU O.SU Analyte concentrations in micrograim_per liter (parts per billion [ppb]). Analyses were performed by Enseco-East of Somerset, New Jersey, using USEPA Method 524.2, Revision 3.0. D Analyte identified at a secondary dilution. J Result is detected below the reporting limit and/or is an estimated concentration. U Compound or element analyzed for, but not detected at the corresponding reporting limit. u Reporting limit raised due to high levels of target analytes. R Result rejected. FR Field replicate of previous sample. GERAGHTY & MILLER. INC ATTACHMENT NO. 3 ANALYTICAL DATA PACKAGES (The contents of this attachment have been provided separately to the USEPA) GERAGHTV & MILLER. INC