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SOIL OVERSIGHT AND SAMPLING SOIL AND GROUNDVATER INVESTIGATION U.S. EPA CONTRACT NO. 68-V9-0002 REVISED BROSSMAN SHORT FORM FOR THE TUTU VELLFIELD SITE ST. THOMAS, U.S. VIRGIN ISLANDS WORK ASSIGNMENT NO: C02048 DOCUMENT NO: TESV-C02048-QA-CLXF OkLJ Vork Assignment Manager Sally OflUnd TES V Regional Manager Scott ASraber / / Date Date '2^ j.1^*™ 'i TES V QA Director Date EPA Remedial Project Manager Caroline Kwan Date QA Officer EPA Region II Date TUT OO6 O288 *64579* 64579 1. PROJECT: 2. PROJECT REQUESTED BY: 3. DATE OF REQUEST: 4. DATE OP PROJECT INITIATION: 5. EPA WORK ASSIGNMENT MANAGER: 6. EPA QUALITY ASSURANCE OFFICER: 7. PROJECT DESCRIPTION Remedial Investigation of Groundvater and Soil Tutu Wellfield Site U.S. Virgin Islands USEPA Region II USEPA Contract No.: 68-V9-0002 Site Number: 2P1D Work Assignment No.: C02048 May 19, 1992 June 2, 1992 Caroline Kwan Laura Scalise Volatile organic contamination of the drinking water aquifer by petroleum hydrocarbons and chlorinated compounds has been documented at the Tutu Wellfield Site on S,t. Thomas, U.S. Virgin Islands. Several facilities in the area use and/or store some form of the contaminants of concern. To date, three potentially responsible parties have been identified: Esso Standard Oil SA., Texaco Caribbean, Inc., and L'Henry, Inc., which operates the 0'Henry dry cleaning facility. Esso and Texaco have joined together to form the Tutu Environmental Investigation Committee (TEIC). Pursuant to an Administrative Order on Consent issued by EPA, TEIC and L'Henry are initiating a remedial investigation to determine the extent of contamination in groundwater and subsurface soil. COM FEDERAL PROGRAMS CORPORATION (CDM FPC) TES V personnel will provide enforcement support for EPA through document evaluation and review, oversight of field activities, and confirmatory sampling and analysis at the Tutu Wellfield site. A. Objective and Scope: CDM FPC will provide field investigation oversight and split sample analyses in accordance with established EPA procedures and the Scope of Work incorporated in the Administrative Order. The oversight team will observe and document all procedures to ensure that the TEIC contractor, Geraghty and Miller (G&M), adheres to established Region II protocol and the EPA approved G&M March 1992 Work Plan and site Field Operations Plan. TES V personnel will accept split-samples from the PRP of approximately 20% of their subsurface soil and groundwater samples. For drummed sludge and and surface soil samples, EPA has requested TES V personnel to accept splits of 100% of the PRP samples. All split samples will be analyzed through EPA's Contract Laboratory Program (CLP) for the same constituents as the PRP samples (see section 7D). -1- TUT OO6 0239 COM FPC will provide sample contninprs for splir samplps anH coordinate the packaging and shipping of all samples to the CLP laboratories. B. Data Usage: The CLP split-sample data will be used to confirm the accuracy of the PRP's analytical data. C. Sampling Locations: Based on Geraghty and Miller's March 1992 Work Plan, G&M will collect a minimum of one subsurface soil sample from each of 30 soil borings, at the site. Seventeen of the borings will be converted to monitoring wells. A map of G&M's proposed boring and well locations is shown in Figure 1. Two rounds of groundwater samples will be collected from the 17 wells. As determined in a recent technical meeting with EPA and the PRP on May 5, 1992, surface soil and drummed solid waste samples will be collected from the area near the Curriculum Building. Background surface soil samples will be collected near outcrop areas upgradient of the Curriculum Building. COM FPC plans to accept splits of six subsurface soil samples, two solid waste samples, two onsite surface soil samples, three background surface soil samples and eight groundwater samples. D. Analytical Parameters and Their Rationale: The principal contaminants of concern in site groundwater are petroleum hydrocarbons, including benzene, toluene, ethylbenzene and xylenes (BTEX), and chlorinated volatile organic compounds. Subsurface soil samples selected by G&M for laboratory analysis will be analyzed for Target Compound List (TCL) volatile organic compounds (VOCs) plus 1,2-dibromoethane, n-propylbenzene, and methyl-tertiary-butyl-ether (MBTE); TCL base-neutral/acid extractables (BNAs); total petroleum hydrocarbons (TPH); and Target Analyte List (TAL) metals and cyanide. Geraghty and Miller will field screen all subsurface soil samples for BTEX, dichloroethylene (DCE), trichloroethylene (TCE) and tetrachloroethylene (PCE) gas using a portable gas chromatograph. Groundwater samples collected by G&M will be analyzed for the same constituents as for subsurface soil listed above. Geraghty and Miller will also collect filtered groundwater samples for dissolved TAL metals analysis. Onsite surface soil samples will be analyzed for EPA's TCL VOCs and BNAs and for TAL metals and cyanide. Background surface soil samples will be analyzed for TAL metals only. Solid waste samples from drums will be analyzed for TCL VOCs only. Per EPA direction, split samples will be analyzed for the same constituents as the PRP, except that splits of filtered groundwater will not be accepted. Analysis for the TCL organic compounds plus 1,2-dibromoethane, n-propylbenzene, and MBTE will be in accordance with the EPA CLP Statement of Work (SOW) for organics, document number OLM01.8 (or current revision). TAL analytes will be analyzed in accordance with the EPA CLP SOW for inorganics, document number ILM01.0 (or current revision). TPH analysis -2- TUT GO6 O29O will be performed in accordance with method 418.1 as stated in Methods for Chemical Analysis of Water and Wastes (MCAWW), EPA-600/4-79-020, revised March 1983. E. Analytes: See Table 1. F. QC Sample Analysis: See Table 2. Duplicates Environmental duplicates will not be collected because the samples accepted per this Brossman Short Form are split samples of the PRP samples. Trip Blanks A. A trip blank will be prepared by the COM FPC TES V team at the start of each day on which aqueous samples will be collected for the analysis of TCL volatiles. Trip blanks are used to determine whether on site atmospheric contaminants are seeping into the sample vials, or if any cross-contamination of samples is occurring during shipment or storage of samples containers. A trip blank consists of demonstrated analyte-free water (based on TCL analysis results below Contract Required Detection Limits) sealed in 40 ml septum vials with no headspace (including bubbles) in the vials. Trip blanks will be preserved as described in section 11.D.3 with HCl to a pH <2. Trip blanks will be kept in close proximity to the samples being collected and maintained at a temperature of 4 degrees celcius. One trip blank will be included with each daily shipment to CLP laboratories that contains aqueous samples collected for TCL volatile organic analysis. Trip blanks will be analyzed for volatile organic compounds only. Control of all trip blanks related to split samples will be the responsibility of the COM FPC TES V field personnel. Certification of blank water quality received in the field will be kept on site and/or will be requested from the supplier and will be filed in the COM FPC TES V project files once field work is completed. Further definition of what constitutes "demonstrated analyte-free water" may be found in the EPA Region II CERCLA Quality Assurance Manual, Revision 1 (October 1989), Section 10-A.2 (pages 59-60). Field Blanks CDM FPC will accept a limited number of random splits of G&M's field blank samples. Field blanks, also known as "rinse blanks" or "equipment rinsate blanks" are used to assess the effectiveness of equipment decontamination. One field blank will be accepted for each equipment type and will be analyzed for the same constituents as the environmental sample splits. Field blanks will be preserved per the requirements for aqueous samples analyzed for these parameters of interest. Field blanks will be collected prior to use of the -3- TUT OO6 O291 decontaminated equipment for sampling. The frequency for field blanks is one per "decon" event, not to exceed one per day, for each equipment type and for each sample matrix. Field blanks are generated by pouring demonstrated analyte-free water over the decontaminated sampling piece of equipment. Field blanks will be collected in a manner that will minimize potential contamination from the ambient air. It is permissible to use the same aliquot of water on all equipment associated with a particular sample matrix for analysis of semi-volatile organics, and inorganic analytes. However, a separate field rinse blank must be collected for each piece of equipment associated with a particular sample media that will be analyzed for volatile organic compounds. Matrix Spike/Matrix Spike Duplicates Matrix spike samples are collected to demonstrate the precision of laboratory analysis. It should be noted that ground water and surface water constitute two distinct matrices. An aqueous matrix spike sample requires the collection of a triple volume in order to perform matrix spike and matrix spike duplicate (MS/MSD) analysis for organics. According to EPA's Region II CERCLA QA Manual, a minimum of one matrix spike sample per matrix must be submitted to the laboratory for every sample delivery group (SDG). An SDG is defined as one of the following: 1. All samples of a RAS or SAS case if the sample number is less than 20 (including environmental duplicates, but excluding QC blanks) and if sampling is completed in less than 14 calendar days. 2. Each group of 20 samples within a RAS or SAS case (including environmental duplicates, but excluding QC blank) if the number is greater than 20. 3. Each 14 calendar day period within a RAS case if the number of samples collected is less than 20. Each 7 calendar day period within a SAS case if the number of samples collected is less than 20. 8. SCHEDULE OF TASKS AND PRODUCTS: The field work associated with the sampling activities is scheduled to begin the week of June 2, 1992, and is estimated to take approximately 18 weeks. Split samples will be collected starting in mid-July when the shallow wells and borings are being drilled. 9. PROJECT ORGANIZATION: The following is a list of key project personnel and their corresponding responsibilities: Sampling Operations Andrew Scano Sampling QC Pam Phillip CLP Coordinator Vasu Desikan Laboratory Analysis Contract Laboratory Program -4- TUT 006 0292 Laboratory QC Data Processing Activities Data Processing QC Data Quality Review Internal Systems Audit Technical Systems Audit Overall QA Health & Safety Coordinator Overall Project Coordination Contract Laboratory Program Andrew Scano Jeniffer Oxford TES V data validation staff TES V QA staff TES V QA staff Rosemary Ellersick Jeanne Li twin Sally Odland 10. DATA QUALITY REQUIREMENTS AND ASSESSMENTS: Data quality will be assessed in terms of accuracy, precision, sensitivity, representativeness, comparability and completeness within each data set and comparison of the split sample data with the PRP's data. The accuracy and precision requirements for the TCL to be performed through Routine Analytical Services (RAS) and Special Analytical Services (SAS) and TAL analyses to be performed through RAS are specified in the EPA CLP Statement of Work for Organics (SOW OLM01.8, or current version) and the EPA CLP Statement of Work for Inorganics (SOW OLM01.0, or current version). In addition to the analysis for volatile organic parameters on the TCL list, analysis will be performed for n-propylbenzene, 1,2-dichloroethane, and MTBE. The method for these organic compounds will be SOW OLM01.8, or current version, and performed through SAS. Historical precision and accuracy requirements will be observed for TPH analyses, to be performed through SAS by the CLP as specified in MCAWW method 418.1 for TPH. Sensitivities required for the CLP analysis of QA samples will be method detection limits from the same cited Statements of Work and the SAS request for TPH. A. Data Representativeness: Representativeness expresses the degree to which the sample portrays the population characteristics of process/environmental conditions at a given location and point in time. Samples from the six soil borings and four monitoring wells (two rounds of sampling yielding 8 groundwater samples) shown in Figure 1 will be split between Geraghty and Miller and the TES V sampling team, or will be collected by G&M and accepted by the TES V sampling team. The samples will be split by equally dividing the contents into two sets of sample containers. Soil samples for analysis of VOCs will be collocated rather than homogenized and divided. Samples will then be sent to different laboratories for analysis. B. Data Comparability: All data will be presented in the units specified in the Contract Laboratory Program's Information For Bidders (IFBs). Split sample data will be compared to the results reported by Geraghty and Miller. -5- TIJT O06 O29-. C. Data Completeness: Completeness is the percentage of all measurements made whose results are judged to be valid. Completeness will be ensured by accepting an adequate percentage of split samples to accomplish project objectives. 11. SAMPLING PROCEDURES: Prior to sampling, and between sampling points, all field equipment will be decontaminated by G&M using the following EPA approved method: o Wash and scrub with low phosphate detergent o Potable water rinse^ o Rinse with W% HN03 (1% for carbon steel implements) o Potable water rinse+ o Methanol rinse* o Hexane rinse* o Thorough Deionized demonstrated analyte free water rinse (at least five times the volume of solvent used) o Air dry o Wrap in aluminum foil * Acid will be Ultrapure grade; solvent will be pesticide grade or better. + Tap water from any municipal water treatment system may be used. The use of untreated potable water supply is not acceptable. During the sampling activity, the TES V team will note the following in the field logbook: o Date, time and weather o Identity of the notetaker o Field personnel/affiliations o Level of personal protective clothing/gear o Schedule for the day o Equipment used (record ID numbers) and calibration information o Sample collection equipment and procedures o Decontamination procedures for the equipment o Sample container and demonstrated analyte-free water shipment lot numbers (as received in the field) o Sample description, depth and location (from two reference points) o Any unusual discoloration or evidence of contamination o Field parameter measurements (such as temp., pH, and specific cond.) o Calculations o Any preservation requirements o Sample volumes and containers used o Sample analysis to be performed o Sample matrix o Sample identification number used by the contractor for their sample and by the TES team for the split sample, o CLP RAS or SAS sample number o Overnight courier airbill number o Deviations from the PRP's approved field operations plan, this Brossman or other problems o Descriptions of any photographs taken -6- TUT OO6 0294 o Notes of conversations with project coordinators. A. Subsurface Soil Sampling 1. Geraghty and Miller will collect subsurface soil samples during soil boring installation in accordance with their March 1992 Work Plan and Field Operations Plan. 2. Split samples for VGA, and TPH soil aliquots will consist of collocated grab samples. 3. Soil samples for all remaining analyses will be homogenized in a stainless steel bowl before filling the containers. 4. All soil samples and splits samples will be carefully logged, packed in coolers with bagged ice sufficient to cool the media to 4 C, and sealed for shipment according to the procedures described in section 12. B. Surface Soil Sampling 1. Geraghty and Miller will collect two surface soil samples from the area around the Curriculum Building and three background samples from areas upgradient of the Curriculum Building in accordance with their March 1992 Work Plan and Field Operations Plan. Background samples will be analyzed for TAL metals only. 2. Split samples for VOA, and TPH soil aliquots will consist of collocated grab samples. 3. Soil samples for all remaining analyses will be homogenized in a stainless steel bowl before filling the containers. 4. All soil samples and split samples will be carefully logged, packed in coolers with bagged ice sufficient to cool the media to 4°C, and sealed for shipment according to the procedures described in section 12. C. Solid Waste Sampling 1. Geraghty and Miller will collect two solid waste samples from drums stored at the Curriculum Building in accordance with their March 1992 Work Plan and Field Operations Plan. Samples will be analyzed for TCL VOCs only. Since the samples may contain high concentrations of organic compounds, they will be analyzed by the CLP method for organic analysis, multi-media, high concentration (SOW for Revision 9/88, including Revision 4/89). 2. Split samples will consist of collocated grab samples. 3. All solid waste samples and split samples will be carefully logged, packed in coolers with bagged ice sufficient to cool the media to 4°C, and sealed for shipment according to the procedures described in section 12. D. Groundwater Sampling -7- TUT OO6 0295 1. A minimum of two weeks after well development, Geraghty and Miller will collect groundwater samples from newly installed monitoring wells in accordance with their approved March 1992 Work Plan and Field Operations Plan. 2. Split samples for VOCs (TCL) plus 1,2-dibromoethane, n-propylbenzene, and MTBE; TCL BNAs; TAL metals plus cyanide; and TPH will be provided by the alternate filling of G&M and COM FPC sample bottles such that representative samples are collected. VGA bottles will be filled first, followed by BNAs, TPH and inorganics. 3. The pH of the VGA sample aliquots will be adjusted to <2 by the dropwise addition of 1:1 HCl to the VGA vials prior to sample collection. The amount of preservative required at each well will be determined by adding HCl to a separate aliquot of equal volume and testing with pH paper. All vials will be checked to ensure zero headspace. 4. The pH of the TPH samples will be adjusted to <2 by adding ^SO^. The H-SO, will be added a small amount at a time, mixed into the sample by tipping, and tested with pH paper. 5. The pH of the metals sample aliquot will be adjusted to <2 by adding HNO-. The HNO., will be added a small amount at a time, mixed into the sample by tipping the bottle, and tested with pH paper. 6. The pH of the cyanide sample aliquot will be adjusted to >12 by adding NaOH. The NaOH will be added a small amount at a time, mixed into the sample by tipping the bottle, and tested with pH paper. 7. All samples and split samples will be carefully logged, packed in coolers with bagged ice sufficient to cool the media to 4 C, and sealed for shipment according to the procedures described in Section 12. 12. SAMPLE CUSTODY PROCEDURES: A. Traffic Reports: A CLP Sample Traffic Report is a four page carbonless form used for RAS samples. A preprinted identification number will be assigned in the field by the TES V team for each RAS sample collected and will be affixed by the TES V team to each container of the sample. An organic traffic report (Figure 2) will be completed for samples receiving organic analyses (VOC and BNA analysis). An inorganic traffic report (Figure 3) will be completed for RAS samples receiving inorganic analyses (metals plus cyanide). A SAS Packing List (Figure 4) will be completed for all SAS samples (TPH; MTBE, n-propylbenze and 1,2-dibromethane; and solid waste TCL VOC analysis). The information that must be completed on the traffic reports and SAS packing lists is detailed in the User's Guide to the Contract Laboratory Program (CLP User's Guide), EPA/540/P-91/002, January 1991, and the Samplers Guide to the Contract Laboratory Program (Samplers Guide), EPA/540/P-90/006, December 1990. Copies of these guides will be on-site. Field QC blanks and matrix spike designated sample splits will be -8- TUT OO6 O296 noted on these forms. B. Chain of Custody Record: To maintain a record of sample collection and transfer for every sample processed, a "Chain-of-Custody Record" will be completed for each cooler shipment. In Region II, the EPA Environmental Services Division form should be used. Figure 5 is an example of this chain-of-custody record which must be secured to the inside of the shipping cooler along with the CLP traffic reports (for samples submitted for RAS analyses) or SAS packing lists. A copy of the custody record is retained for the FPC TES V files. Shipping coolers will be secured with nylon fiber strapping tape or its equivalent and custody seals (see Figure 6) will be placed across cooler openings so that the cooler may not be opened without breaking the seals. A mailing label addressed to the laboratory will also be attached to the cooler and protected by clear tape as back-up to the courier airbill so that coolers may not need to be opened by courier staff in the event that the airbill is separated from the cooler. The PRP contractor will be required to sign COM FPC's custody form as the sample collector. Each time the samples are transferred to another person, signatures of the persons relinquishing and receiving them, as well as the time and date of transfer will be completed in the appropriate spaces on the chain-of-custody record. The PRP contractor will relinquish the sample to the TES V sampler (COM FPC) who will be the second sampler. Samples will be shipped from the field directly to the laboratories designated to perform the analyses via Federal Express or an equivalent overnight courier. Samples will be sent to the laboratory from the field within 24 hours of sample collection. All courier receipts and/or paperwork associated with shipment of the samples will serve as a custody record for the samples while they are in transit from the field to the laboratory. Custody seals should remain intact during this transfer. When the samples are delivered to the laboratory, signatures of the labortory personnel receiving them and courier personnel relinquishing them will be completed in the appropriate spaces on the chain-of-custody record. This will complete sample transfer. It will be the CLP laboratory's responsibility to maintain internal log books and records that provide a custody record throughout sample preparation and analysis. To track field samples through data handling, COM FPC will maintain photocopies of all traffic reports, SAS packing lists and chain-of-custody records. When responsible for sample custody, field personnel should keep in mind the definition of sample custody according to the EPA Office of Enforcement and Compliance Monitoring National Enforcement Investigations Center (NEIC) Policies and Procedures (May 1986) that states that a sample is under custody if: 1. it is in one's possession, or 2. it is in one's view, after being in one's possession, or 3. it is locked up after being in one's possession, or -9- TUT 006 0297 4. it is in a designated secure area. C. Sample Labels and Tags: One numbered adhesive RAS label from the strip (Figure 4) or a hand written label for SAS samples (and the additional HS/MSD bottles filled for aqueous RAS organic extractables) is affixed to each container making up the sample. To protect the label from water and solvent damage, each label is covered with clear waterproof tape. For samples requiring decontamination, the self-adhesive sample labels must be completely covered with clear mylar tape prior to sampling. The sample labels permanently identify each sample collected and link each sample component throughout the analytical process. In addition to the preprinted sample identification number, each split sample container for CLP analysis will be identified with a sample tag (Figure 6). These sample tags are retained by the CLP laboratories as physical evidence of sample receipt and must therefore be signed by the sampler, which in the case of split samples is the TES V oversight contractor (COM FPC) sampler accepting the split sample. The sample tag will contain an abbreviated summary of the field logbook entry for the sample. The information that must be entered on the sample tag is detailed in the CLP User's Guide and listed below. o Site spill number (do not provide the site name or address) o CLP case number or SAS number o RAS of SAS sample number o Date and time of collection o Station number/location o Sampler signature o Sample type (composite or grab) o Sample matrix o Preservative added and type o Type of analysis required. D. Field Notebooks: A final element in the documentation process will be the completion of a formal field notebook by TES V personnel. The field notebooks will be maintained by the TES V team and will be stored in the TES V document control systems. All entries will be made in accordance with the TES V requirements for maintaining field notebooks as detailed in the Camp Dresser and McKee Inc. (COM) Site Investigation Procedures Manual, SOP #5621004. A copy of this SOP will be available on-site. The information that will be recorded in the field notebooks for each sample collected by the Contractor is described in Section 12, Sampling Procedures. E. Sample Bottles: CDM FPC will purchase pre-cleaned sample containers which meet EPA specifications. These bottles are pre-cleaned in accordance with OSWER -10- TUT OO6 O298 Directive number 9240.0-05 and 0^ fpsfpd arrnrrlinp; to prescribed procedures to ensure that no contamination exists that might affect sample data. QC screening procedures include container cleaning by lot group; each lot group is assigned a unique identifying number, which is permanently affixed to each container. Clean, empty bottles are shipped to users in protective cardboard cartons. F. Sample Handling, Packaging, and Shipping: When sent by common carrier, the packaging, labeling and shipping of hazardous wastes and substances is regulated by the U.S. Department of Transportation (DOT) under CFR 49. Samples obtained at uncontrolled hazardous waste sites are classified according to pollutant concentration. "Low Level" samples are generally dilute and are usually collected from areas surrounding a spill or dump site (i.e., offsite samples from soils, rivers, lakes, etc.). "Medium Level" samples are generally collected on-site, in areas of moderate dilution by normal environmental processes. It is anticipated that contaminant concentrations in all samples collected from the Tutu site will range between low level and medium level. All samples will be packaged and shipped according to the following procedures detailed in the current (January 1991) CLP User's Guide and Samplers Guide (see previous references). C Samples will be kept on ice to maintain a temperature of 4o . The samples will be shipped within 24 hours of collection via an overnight carrier. Each sample label will be covered with clear waterproof tape to protect it from water and solvent attack. A custody seal (Figure 6) is to be placed over the lid of all sample bottles and also the shipping cooler, before shipping it to the laboratory. This will ensure that the samples are not opened prior to their arrival at the laboratory. G. Sample Shipment Coordination: To enable the Sample Management Office (SMO) to track the shipment of samples from the field to the laboratory and ensure timely laboratory receipt of samples, the TES V team will notify the SMO (phone number: (703) 684-5678) immediately following all sample shipments, and provide the following information: o Sampler name and phone number o Case number and RAS or SAS number o Site name/code o Exact number(s) and matrix(ces) and concentrations of samples shipped o batch numbers (dioxin only) o Laboratory(ies) samples were shipped to o Carrier and airbill number(s) for the shipment o Method (e.g., overnight, two-day) o Date of shipment o Any irregularities or anticipated problems with the samples, including special handling instructions, or deviations from established sampling procedures. o Suspected hazards associated with the samples or site. -11- TUT 006 0299 o Status of the sampling project (e.g., final shipment, update of future shipping schedule). H. Sample Trip Reports: A sample trip report is required to be completed for each case number and must contain all the information as shown below. All blanks and duplicates must be clearly indicated. o Site number o Sampling date o EPA case number and RAS or SAS number o Site location/name o Sample description o Names, addresses of laboratories receiving samples and sample types going to those laboratories. o Sample dispatch data (e.g., Federal Express airbill number(s)) o Names, organization, affiliation and duties of onsite sampling personnel o Additional comments (samples types, totals, blanks, etc.) o Name of preparer and date of report o Approval signature and date. This trip report will be sent directly to the Regional Sample Control Center (RSCC) within 10 days of final sample shipment with a copy to the TES V CLP coordinator. 13. CALIBRATION PROCEDURES AND PREVENTATIVE MAINTENANCE: A. Field Equipment: Each piece of TES V equipment used for measuring, monitoring, analytical purposes is calibrated and maintained periodically to ensure accuracy within specified limits. Calibration and maintenance procedures and the frequency at which these procedures should be applied are detailed in the COM Field Equipment Operation, Maintenance, and Calibration Manual (FEOMC Manual). A copy of this document will be onsite. TES V field equipment undergoes calibration and maintenance by qualified personnel before and after every field activity. If an instrument is to be in the field for longer than four weeks, it is returned to the Region II equipment room to undergo full calibration and maintenance. Where applicable, instrument calibration is field checked. The following equipment will be used by the TES V team at the Tutu site: Instrument SOP Reference HNu Photoionization Detector (PID) FEOMC Manual, Section 1.0 A field equipment status report is kept for each piece of field equipment and kept in a Region II Log Book. The Log Book is stored at the COM FPC Regional office. These reports contain the following information: -12- TUT 006 o Date of calibration and Hnte of last maintpnance o Initials of person performing the calibration and/or maintenance o Accuracy prior to and following calibration and/or maintenance o Notations on equipment failures. B. Laboratory Equipment: Calibration procedures and preventative maintenance for laboratory equipment is the responsibility of the CLP lab selected to analyze the samples. 14. DOCUMENTATION, DATA REDUCTION, AND REPORTING: A. Documentation: This QAPP and the Geraghty and Miller Investigation Work Plan will be available to COM FPC personnel in the field. Each sample submitted for analysis will be properly documented to ensure timely, correct, and complete analysis for all parameters requested and to support the use of analytical data in potential enforcement actions. The following documentation will be submitted: o Organic and inorganic sample traffic reports o Chain of Custody Records o Field logbooks o Sampling labels o SAS packing list (where appropriate). B. Data Reduction and Reporting The CLP will be responsible for preparing the analytical data packages for organic analysis and providing this information to the SMO. SMO will then send the package to the RSCC for data validation. Data reduction will consist of summarizing the data collected during the field work. The data will be used to prepare a report summarizing the analytical results and notes taken during the field work. 15. DATA VALIDATION: Analytical data will be validated by the TES V team by the following EPA Region II standard operating procedures: 1. SOP Number HV-2: Inorganic Data Validation, Revision 11, January 1992. 2. SOP Number HW-6: Organic Data Validation, Revision 8, January 1992. 16. SYSTEM AUDIT: A field technical and/or internal system audit may be conducted by the COM -13- TUT OO6 0301 FPC QA staff during the course of this assignment. If so, each audit will be documented in a report discussing any observed deficiencies for each phase of work. If needed, a Corrective Action Request will be completed and sent with the audit report. Upon receipt of a satisfactory response, an Audit Completion Notice will be issued. If no deficiencies are noted, the original audit report will serve as the Audit Completion Notice. Reports are sent to the audit file with copies to the audited entity, COM FPC management and EPA. System audits may also be performed or arranged by EPA. Laboratory performance audits are the responsibility of the CLP and EPA. 17. CORRECTIVE ACTION: If a nonconformance or deficiency is identified during a systems audit, and has not been corrected during the audit, corrective action will be initiated by the TES V Regional QA Coordinator (RQAC), as appropriate. The TES V Quality Assurance Director (QAD) will be responsible for filing a report of the audit along with a Corrective Action Request Form if any nonconformances were noted during the audit. The TES V QAD will also be responsible for ensuring that corrective action is taken and will forward the report to the audited entity, COM FPC TES V management and EPA. The COM FPC TES V team will be responsible for reporting all suspected technical nonconformances. Any staff member who discovers or suspects a nonconformance in an approved document shall inform the TES V work assignment manager (WAM), who is responsible for determining if a corrective action is required. The WAM shall ensure that no additional work, which is dependent on the nonconforming activity, is performed until the nonconformance report is corrected. Oversight personnel should maintain a logbook in which observations of poor practices or discrepancies from the governing plans on the part of the PRP contractor should be noted. The EPA WAM should be notified of such findings by phone. 18. REPORTS: The EPA will be provided with all the data gathered during this field activity. During field activities, COM FPC will provide weekly written or verbal reports to EPA detailing PRP activities and any observed discrepancies from the approved sampling plans. An overall field summary report will be provided to EPA at the end of each period of field work. Laboratory results from split samples will be evaluated and presented to EPA in the form of a Letter Report, detailing QA/QC measures taken during sampling/field activities. Any report containing measurements will contain a QA section which includes data quality objectives and parameters, the results of any audits peformed by the FPC TES V QA staff and/or EPA, and any deviations from the EPA approved guidance documents (such as this Brossman Short Form). Such a report will undergo QA review by the RQAC or her designee after it has received technical review. -U- TUT OO6 TABLE 1 PARAMETER TABLE FOR TES V SPLIT SAMPLES SUBSURFACE AND SURFACE SOIL INVESTIGATION TUTU WELLFIELD SITE ST. THOMAS, U.S. VIRGIN ISLANDS ANALYSIS VOCs EST'D MATRIX NO OF SAMPLES* 8 soil ANALYTICAL METHOD Ref. 1 HOLDING TIME PRESERVATIVE VTSR ** Cool to 4°C 10 days SAMPLE CONTAINER 2x40-ml glass vials/ Teflon septa MTBE, n-Propyl- benzene + 1,2-Dibro- moethane soil Ref. 1 Cool 10 days to 4°C 2x40-ml glass vials/ Teflon septa BNAs soil Ref. 1 Metals Metals + Cyanide TPH soil soil Ref. 2 Ref. 2 soil 418.1(3) Cool to 4°C 10 days to extraction/ 40 days to analysis Cool to 4°C 6 months Hg-26 days Cool to 4°C 6 months Hg-26 days Cn-12 days Cool to 4°C *** 26-days IxSoz wide-mouth glass jar IxSoz wide-mouth glass jar IxSoz wide mouth glass jar IxBoz wide-mouth glass jar * - Based on splitting 20% (6) of the PRP subsurface soil samples and 100% (5) of the PRP surface soil samples. The 2 onsite surface soils will be analyzed for TCL VOCs, TCL BNAs and TAL metals only; the 3 background surface soil samples will be analyzed for TAL metals only. ** - From verified time of sample receipt *** - The extraction of soil for TPH analysis is to be performed according to EPA/Army Corps of Engineers approved Oil and Grease Procedure for Sediment Samples given in Attachment I. After extraction proceed to Step 7.6 in Method 418.1 for TPH analysis -15- TUT 006 TABLE 1 PARAMETER TABLE FOR TES V SPLIT SAMPLES GROUNDWATER INVESTIGATION TUTU WELLFIELD SITE ST. THOMAS, U.S. VIRGIN ISLANDS ANALYSIS ESTIMATED MATRIX NO. OF SAMPLES* VOCs 8 aqueous MTBE, 8 aqueous n-Propyl- benzene + 1,2-Dibro- moe thane BNAs 8 aqueous Metals 8 aqueous Cyanide 8 aqueous TPH 8 aqueous ANALYTICAL PRESERVATION METHOD HOLDING TIMES VTSR ** Ref. 1 Cool to 4°C 1:1 HCL to pH<2 (a) 10 days Ref. 1 Cool to 4°C 1:1 HCL to pH<2 (a) 10 days Ref. 1 Cool to 4°C 5 days to extraction/ 40 days to analysis Ref. 2 Cool to 4°C HN03 to pH<2 6 months Hg - 26 days Ref. 2 Cool to 4°C NaOH to pH>12 12 days 418.1(3) Cool to 4oC 1:1 H2SO, to pH<2 26 days SAMPLE CONTAINERS 2x40ml glass vials/ Teflon septa 2x40ml glass vials/ Teflon septa 4xl-liter amber jars Ixl-liter poly bottle Ixl-liter poly bottle Ixl-liter amber jar * - Based on splitting 20% of the PRP samples ** - From verified time of sample receipt (a) If sample acidification causes effervescence, the sample will not be acidified but will be cooled to approximately 4 C. In this event, the holding time is 7 days from the time of sampling. -16- 0304 TART.F, 1 PARAMETER TABLE FOR TES V SPLIT SAMPLES SOLID WASTE INVESTIGATION TUTU WELLFIELD SITE ST. THOMAS, U.S. VIRGIN ISLANDS ANALYSIS ESTIMATED NO. OF SAMPLES* VOCs 2 MATRIX solid waste ANALYTICAL METHOD Ref. 4 PRESERVATION HOLDING TIMES VTSR ** Cool to 4°C 10 days SAMPLE CONTAINERS 2x4oz wide- mouth glass jars with teflon-lined septa cap * - Based on splitting 100% of the PRP samples ** - From verified time of sample receipt References 1. "Statement of Work for Organic Analysis, Multi-Concentration." USEPA Contract Laboratory Program, OLM01.8 (or current revision). 2. "Statement of Work for Inorganic Analysis, Multi-Concentration." Contract Laboratory Program, ILM01.0 (or current revision). USEPA 3. Methods for Chemical Analysis of Water and Wastes: EPA-600/4-79-020, revised March, 1983. 4. "Statement of Work for Organic Analysis, Multi-Media, High-Concentration." Revised 9/88, including Revision 4/89. -17- TUT OO6 03O5 TABLE 2 QA/QC SAMPLE SUMMARY TABLE SOIL AND GROUNDVATER INVESTIGATIONS TUTU WELLFIELD, ST. THOMAS, U.S. VIRGIN ISLANDS Sample Type Matrix Parameter Invest!- Matrix Field Trip Total gative spike blank blank Aqueous VOCs 8 2** 2 4 16 Aqueous MTBE, n-Pro- 8 2 2 A 1 6 pylbenze, + 1,2-dibromo- ethane Aqueous Extractables 8 2 * * 2 - 1 2 (BNAs) Aqueous Inorganics 8 2 2 - 1 2 (Metals + Cyanide) Aqueous TPH Soil VOCs Soil Soil Soil Soil Soil Solid Waste MTBE, n-Pro- pylbenze, + 1,2-dibromo- ethane BNA Extractables Inorganics (metals) Inorganics (metals + cyanide) TPH VOCs 6 8 5 6 6 2 8 8 6 2 * 3 * 2 10 11 8 11 6 8 * 6 * 2 -18- TUT OO6 0306 NOTES FOR TABLE 2 1) Based on accepting splits of 20% of the PRP's subsurface samples and 100% of the PRP's surface soil samples. Two randomly selected field blanks will be split with the PRP for subsurface soils and one for surface soils. 2) Assumes two groundwater sampling events with split samples accepted on 2 days for each event. * The lab will analyze a matrix spike and matrix spike duplicate from existing soil or sediment sample volume. ** Triple volume must be collected (volume includes investigative sample). Because the entire sample is consumed in analysis, a laboratory duplicate will be collected for every sample delivery group for aqueous TPH analyses and labeled as a lab duplicate. 006 0307 \ frtH^OV WQMTOHMC «C NC «l «eu. ' GERAGHTY & MILLER, INC. SITE PLAN ' V C E S~A"3\ '\VESTiGATiO\ CVAS. w.S. V'RG N IS_A'OS I TUT' 006 O3O9 -i lUt ryPiorj POBollt .1 Protection AQ^| Sample Mencgemi Ifn Alwndrif,. VA 22313 FIS 447 2490 IOMC4) Inorganic traffic Report <R)r CLP (J*9 Only) V|M of AdMTr (Chtck orw) ENF ~ <R.O ~ RA EH _ O4M _ RO ESI PA RIFS Soperfend ProgrwH S15I Acme. Co. S«mplw (Nwn*) Joan Sampler 1 Slvp to /OO 4 O«l* Shippwt 1 MfbM NurntMt C»llM fed Ex t)oubl« volum* i«qulf*d lor mtfrta Ship mtrturn »nd Wgh conc«nlr*Uan t*m|>**t In |MM cent C«M Number ioi a i SASNo (HcppMcsbi*) & Sampto OtmittiHoii fEnrcr In Cofemn x; 1. Sud«o«WM«r 2. Ground Water 3. LaactoU 5 SoN/S«>m«nl 8 OH(SAS) 7. WiJto(SAS) 8. Olhec (SAS) (Specify) ;ui "i ENVIRONMENTAL PROTECTION AGENCY r.LP Sample Management Office P.O. BoillS - Alexandria, Virginia 22313 Phone-. 703/357-2*90 - FTS/W7-2**) SAS Number 1000 -A SPECIAL ANALYTICAL SERVICE PACKING LIST Sampling Office: fStQipr^ TZ. J Sampling Contact: Jot SOJVA^ItV (name) i*i-*)5^-i^i*4 (phone) Sampling 1 il|>\- H Date Shipf — uj* ——— >ate(s): |4l^ ted: ?i Site Name/Code: ^01 Ship To: SAS LA6 »oo Mairt SnSnU- A^-to** , Co W^S" Ann! Ji*i Srtiih For Lab Use Only Date Samples Rec'd: Received By: 1. 2. 3. *. 3. ft. 7. S. 9. 10. 11. 12. 13. 1<*. 13. Sample Numbers \cccA - oi IOOOA • 0* looc 4 • oi IOCC4 -od 10004 . o«^ lOftC A - 01, 16. 17. IS. 19. 20. Sample Description Analysis, Matrix, Concentration Sample Condition on Receipt at Lab For Lab Use Only White • SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Gold - Lab Copy TUT O06 0311 IX te ^ ^ I v *r IMVttOWMINTAL MOTfCTtON AOIWCT - UWOM • Environmental Services Division totsoM. NIW mm «itir | *»•• 1 . I •' jc,«..« *»•••< . _ . - •' 0**<nM>» •! (•••tat C FIGURE •*"- TUT O06 031 © i £ CIP Sample No Monlh/Oay/Yoai |i •^^^^^^••••M o "eT£ Preservative: . s Yes D No C !° Type | a ANALYSIS y volatile Oroanies — • Orotniei-BNAs £ PctnetMBVPCBs ^ i Cyaniot i : •r 2J.7.8-TCOO 1 M I 5 1 I : I 1 I : 1 3 ' Rtmims: 0z § i I Tag NO. UD SampH) No. "02 1998 REGION 2 • si-uurmi ^^^^^^m^^a IAMPLI NO. IDAIt SIGNATUIIE MINT MAMt AND lllLfc (Inyatur. yliwfr* a TKAni-nJ .,••••" v UNITED STATES , ^V • ENVIRONMENTAL. PROTECTION AGENCY 1 •» i OFFICIAL tAMf»LE SEAL 1.3BJ ''. «o.*c ! 1 "Uf OO6 0313 COM FEDERAL PROGRAMS CORPORATION Figure 6 Sample Tag/Custody Seal Attachment I EPA/Army Corps of Engineers Oil and Grease Procedure for Sediment Samples TUT Procedure for Sediment Samples (Sir) The procedure for determination of oil and grease in sedi- ment samples is similar tc that used to quantify oil and grease ir. water sar.tle;. The sample is extracted with Freer, and the extractable material is quantified. As indicated in Figure 3-39, a moist sediment sample must be used as a dried sample will yield low results. Because of the operational definition of the oil and grease procedure and the lack of precision associated with the test, it is recommended that cor.- ditions of sampling, sample pretreatment, and analysis be standardized 3 tr.e :.na_ data. i .-.ethoz _: rrecr. rjctraction Apparatus Extraction apparatus, Soxhlet Vacuum pump or other source of vacuum Extraction thimble, paper Ir.frs.r6i srectrtrhotor.eter or balance reagents Marr.esium sulfate mcnohydrate: prepare MgSOu • H20 by drying a thin layer of MgS!* • TK:- overnight ir. an oven at 1C2 CC. Frerr. [ l,l,2-trichloro-l,2,2-triflucroethane) , boiling point *7°C. The solvent should leave no measurable residue on evaporation. Heii- still if necessary. C-r ease-free cotton: extract nonabsorbent cotton with Freor.. •Inrwr. :il reference standard: accurately weigh about 0.05 g of known oil directly into a 100-ml volumetric flask. Add 80 ml Freor. and dissolve the oil. If, as in the case of a heavy fuel oil, all the oil does not go into solution, let stand overnight. Filter through a Whatman No. '-C filter paper into a second 100-ml volu- metric -flask and dilute to volume with Freor.. "JrJcnowr. oil reference standard (10 ul = 7.6? mg oil): pipet 15 ml n-hexadecane, 15 ml isooctane, and 10 ml benzene into a 50-ml glass-stoppered bottle. Assume the specific gravity of this mixture to be 0.769 and maintain the integrity of the mixture by keeping the bottle stoppered except when withdrawing aliquots. Weigh a 20.C-r sample of ncist sediment (SID) in a 15C-ml 3-231 TUT OO6 O315 beaker. (The solids content of the sample should be known in advance er" determined en a separate sar.ple aliquot.} Acidify the samrle with ecr.c. t: make a -uniformly smooth paste that is spread on the beaker wall. All:-.- to stand 15 to 2- min until solidified. Remove the solids and grind in a porcelain mortar. The use of a desiccated, uniformly ground sample improves the efficiency of the extraction process. Add the ground sample to a paper extraction thimble. The beaker and mortar should be wiped with a small piece of filter rarer that has been soaked in Freon. Add the filter paper to the paper thimble. "ill t:.t thl:.."_le with glass wool or small glass beads. Extract the pre- pared sample with Freon in a Scxhlet apparatus at a rate of 20 cycles,'hr for - hr. If the final extract is turbid, filter the sample through grease-free cotton into a clean flask. Rinse the initial sample con- tainer and the cotton with Freon and add the washing to the filtered sample, let ermine the oil and grease concentration of the extract by either infrared spectrophotometry (aj or graviiaetry (b_). The infrared method would be preferred because it is generally -ore precise; partir- •;l3.rl;- =t lev oil and grease concentrations. _a. Infrared spectre-photometry. 1 '2 Quantitatively transfer the sediment extract to a convenient size volumetric flask and dilute to volume with Freon. Prepare calibration standards using either the known cil reference standard or the unknown cil reference standard. (A known oil is defined as the only grease and/or cil component in the samples being analyzed. An unknown oil is defined as the grease and/or oil component(s N in the sample being analyzed for which standard prepara- tions are not available.) Transfer required amount? of the appropriate reference material into lOC-ml volu- metric flasks using micrcliter pipettes. Dilute to volume with Freon. The most appropriate pathlength for the quartz cells to be used in the spectrophotcmetric determination is determined by the expected sample concentration. The following information is presented as a guide for selecting cell length: 3-285 TUT 006 0316 Pathlength, cm Expected Range, mg 1 u - uO 5 Q.5 - 8 10 0.1 - U Based or. observed ranges of oil and grease in seiirer.t r, it nay be necessary to dilute the sample extracts tc the working ranges indicated above. Scan the standards and samples from 32CC to 2" TCC cm"1 using a recording infrared spectrophotoneter. Freon should be used in the reference bean of a dual bean instrument or to zero a single beam instrument. The absorbance of the 2930-cm"1 peak should be used to con- struct a standard curve. Gravimetry.1 The gravimetric determination of oil and grease does not require dilution of the samples. However, the procedure is considered less precise than the infra- red determination because the method is subject to posi- tive sulfur interference and greater uncertainty at low oil and grease concentrations. To implement the method, quantitatively transfer the sediment extract to a tared distilling flask. Rinse the extract container with Freon and add to the distilling flask. Distill the Freon from the extraction flasks using a water bath at 70°C. After the solvent has beer, evaporated, place the flask on a warm stear. bath for 1; min and draw air through the flask by means of an applied vacuum for the final 1 min. Cool in a desiccater for 30 min and weigh. The gain in weight is due to oil and grease if the solvent is free of residue. Tabulations Select the appropriate method and calculate the oil and grease : er.tr at ion based on the method of quantification that was used. a_. Infrared speetrophotometry. When colorimetry is used, prepare a standard curve by plotting measured absorbance vs. oil and grease concentration of the standards. Compare the abscrbance of the Freon extract tc the standard curve to determine the oil and grease concen- tration. Calculate the oil and grease concentration C + G of the original water sample as follows: 0 . G m g / k g ( w e t weight)- (*)(V)(1000) (Y) '•"•> t^ •^~~* 1 C + G ing/kg (dry weight) = ' " / _ (gH* 3-286 TUT OO6 O317 where X = ocrcer.trat i or. cf oil ar.f crease ir. the Freer, extract, ng/x g = wet weight cf sediment extracted, g % S = percent solids in the sediner.t sample (expressed as a decimal fraction! Gravir.etry. When the amount of oil and grease is determined by weighing the material extracted, the oil and grease concentration cf the sedisent sarple is calculated as fellows: + G ing/kg (wet weight) = (g) 3 mg'kg (dry weight) = (A ",~g}~^l\"'~ where A = weight of tared flask and oil and grease residue, nig B = weight cf tared flask, rg C = calc-olated residue based en Freer, flask, rzi g = wet weight of sediment extracted, g % S = percent solids in the sediment sanple '•stressed as a decimal fraction; 3-237 TUT OO6 0313 References American Put lie Health Association. Standard Methods for the Exami- r.s.ticr. of Water ar.i Wastevater Including Bettor". Sediments ar.i Sludges, l-.tr. Edition. A?HA; New York, New York. 1193 F- ^-9^6,. Environmental Protection Agency. "Manual of Methods for Chemical Analysis cf Water and Wastes." Methods Development and Quality Assurance research Laboratory, National Environmental Research Center; Cincinnati, Ohio. 298 p. (19T-). Zisalv;, '.. , Guard, H., Hirsch, S . , and !;g, J. "Assessment and Significance of Sedinent-Associated Oil and Grease in Aquatic Environments." Naval Biosciences Laboratory, Naval Supply Center; Cakland , California. Technical Peport D-"T-26; U. S. Amy Enginee Water-ways Experiment Station, CE; Vicksb-urg, Mississippi. 1^-5 p. 3-288 Tu"f 006 03 J. 9 PETROLEUM HYDROCARBONS, TOTAL RECOVERABLE Method 418.1 (Spectrophotometric, Infrared) CTORET NO. 45501 1. Scope aad Application 1.1 This method is for the measurement of fluorocarbon-113 extractable petroleum hydrocarbons from surface and saline waters, industrial and domestic wastes. 1.2 The method is applicable to measurement of light fuels, although loss of about half of any fuoiiac preseat during the extraction manipulations can be expected. 1.3 The method is sensitive to levels of 1 mg/1 aad less, aad may be extended to ambient monitoring. 2. Summary of Method 2.1 The sample is acidified to a low pH (< 2) and serially extracted with fluorocarbon-113 in a separatory funnel. Interferences are removed with silica gel adsorbant. Infrared analysis of the extract is performed by direct comparison mith standards. 3. Definitions 3.1 As in the case of OO aad Grease, the parameter of Petroleum Hydrocarbons is defined by the method. The measurement may be subject to interferences and the results should be evaluated accordingly. 3.2 Oil aad Crease is a measure of biodegradable animal greases and vegetable oils along with the relative Bon»biodegradablt mineral oils. Petroleum hydrocarbons is the measure of only the miaeral oils. Maximum information may be obtained using both methods to measure and characterize oQ aad grease of all sources. 4. Sampling aad Storage 4.1 A representative sample of I liter volume should be collected in « glasa book. Because- ; tbndhcttoffofa composite tampk is deJayc*g 5.1 Scpantofytaad. 3000 ml, with Teflon stopcock. 5J niter piper. Whatman No. 40, II cm. 5 J Infrared spectrophotometer. scanning or fixed wavelength, for measurement around 2950caV*. 5.4 5J Magnetic stirrcr. with Teflon coated stirring bars. 6. Reagents 11 Hydrochloric acid, 1:1. Mix equal volume of cone HO and distilled water. tawed 1971 4ILM TUT 006 0320 6.2 F1uorocarbon«M3.(l,l^*ihehJero»1^2>thfluroethafie),b.p.4rC 6.3 • Sodium sulTatc, anhydrous crystal 6.4 Silica f el, 60-200 mesh, Davidson Grade 9SO or equivalent Should contain 1-2% water as defined by residue test at 130*C Adjust by overnight equilibration if needed. 6.5 Calibration mixrum: 6-3.1 Reference oil: Pipet 15.0 ml n-heiadecanc. 15.0. ml jaooctaac, and 10.0 ml chlorobenzene into a 50 ml glass stoppered bottle. Maintain the integrity of the mixture by keeping stoppered except when withdrawing aiiquota. 6J.2 Stock standard; Pipet 1.0 ml reference oO (6.5.1) into a tared 200 ml volumetric flask and immediately stopper. Weigh and dilute to volume with nuorocarboa*! 13. 6J J Working standards: Pipet appropriate volume* of stock standard (6J.2) into 100 ml volumetric flasks according to the cell pathlength to be used. Dilute to volume with fluorocarboa-113. Calculate ceaccntratioa of standards from the stock- standard. 7. Procedure 7.1 Mark the sample bottle at the water meniscus for later determination of sample volume. If the sample was not acidified at time of collection, add 5 ml hydrochloric acid (6.1) to the sample bottle, After mixing the sample, check the pH by touching pH*sensitive paper to the cap to insure that the pH is 2 or lower. Add more acid if necessary. 7.2 Pour the sample into a sepantory funncL . . . 7J Add 30 ml fluorocarbon-l 13 (6.2) to the sample bottle and rotate the bottk to rinse the sides. Transfer the solvent into the scparatory fennel Extract by shaking vigorously for 2 minutes. Allow the layers to separate 7.4 Filter rhe solvent layer through a funnel containing soIveaMnoistened filter paper into a 100 ml volumetric flask. NOTE I: An emulsion that fails to dissipate can be broken by pouring about I g sodium sulfate (6 J) into the filter paper COM aad slowly draining the emuhuoa through the salt. Additional I g portions can be added to the cone aa required. 7J Repeat (7J and 7.4) twice more with 30 ml portions of fresh solvent, combining all solvent into the volumetric flaakv 7.6 Rinse the Up of the sepantory njnnel.Djtcr paper, and the funad with a total nf 5-10 ml KJQeat irthccatnctir- ropriateportioBC/thesaa^toalOOoUvcJum«tricir>ddnutetovoh«n«> 7.7 D*sca^a*M5-tOmJsoirtoftfronrtlttvofeactrkflast stirring bar; stopper the volumetric flask, aad stir the solution for • s»aumvmc/5minc** TUT OOA O321 7.1 Select appropriate working standards and eell paihlengih according to the following table o/approximate working ranges: aMsBf Calibrate the instrument for the appropriate cells using a aeries of working standard* (6JJ). It is not necessary to add silica gel to the standards. Determine absorbanee directly for each solution at the absorbancc maximum at about 2930 cm*1. Prepare a calibration plot of absorbanee vs. mg petroleum hydrocarbons per 100 ml solution. 7.9 After the silica gel has settled in the sample extract, fill a clean eell with solution and determine the absorbancc of the extract. If the absorbanee exceeds O.S prepare an appropriate dilution. NOTE 2: The possibility that the absorptive capacity of the silica gel has been exceeded can be tested at this point by adding another 3.0 f silica gel to the extract and repeating the treatment and determination. 7.10 Determine the concentration of petroleum hydrocarbons in the extract by comparing the response against the calibration plot. Calculations 1.1 Calculate the petroleum hydrocarbons in the sample using the formula: rag/1 Petroleum Hydrocarbons m * j) p aawtj *m^tff*nikamHtfi\i^miu4*HuaH*tnuib*mltontotk*Q.\OL * D« extract dftrtJon actor; if i V • vohtm ofaampk, fa feat*. t.I Prarisfc»aflda»eiiijdauaresrtavaflabkatthisttae. -u;s< TUT OO6