STANDARD OPERATING PROCEDURE AQ-1 SEQUENTIAL EXTRACTION OF METALS

Transcription

1 STANDARD OPERATING PROCEDURE AQ-1 SEQUENTIAL EXTRACTION OF METALS

2 STANDARD OPERATING PROCEDURE ACKNOWLEDGEMENT FORM Project Number: Project Name: Newtown Creek RI/FS My signature below certifies that I have read and understand the procedures specified in this Standard Operating Procedure. Date Name (print) Signature Company Newtown Creek RI/FS

3 Date Name (print) Signature Company Newtown Creek RI/FS

4 SCOPE AND APPLICATION This Standard Operating Procedure (SOP) is applicable to the preparation of sequentially extracted sediment samples, which will be performed as part of the Remedial Investigation/Feasibility Study (RI/FS) for Newtown Creek. Selected samples will be subjected to sequential extraction analysis to quantify the target analyte list (TAL) metal speciation. The extraction procedure is designed to release fractions from a sample according to their availability by subjecting the sample to a series of chemical treatments targeted at specific chemical forms. A simplified procedure consisting of five extraction steps will be performed yielding the following fractions: 1) exchangeable, 2) carbonate bound, 3) reducible fraction (iron or manganese oxide bound), 4) oxidizable (sulfide or organic matter bound), and 5) residual. The TAL metal concentrations will be determined for each of the fractions collected. Details of the sequential extraction procedure were adapted from methods published by Tessier et al. (1979) and Zimmerman and Weindorf (2010). Procedures for sequentially extracting sediments outlined in this SOP are expected to be followed. Substantive deviations from the procedures detailed in this SOP will be summarized in the Data Summary Report. HEALTH AND SAFETY WARNINGS Health and safety issues for work associated with this SOP are addressed in the Environmental Geochemistry Laboratory Chemical Hygiene Plan (CHP; Anchor QEA 2012). PERSONNEL QUALIFICATIONS Personnel executing these procedures will have read, be familiar with, and comply with the requirements of this SOP, the CHP (Anchor QEA 2012), the Phase 2 Remedial Investigation Work Plan Volume 1 (Anchor QEA 2014a), and the corresponding documents (i.e., Phase 2 Quality Assurance Project Plan and Phase 2 Field Sampling and Analysis Plan Volume 1; Anchor QEA 2014b and 2014c, respectively). Staff in the research facility have minimal contact with sediment and are not required to have any health and safety certifications. Newtown Creek RI/FS

5 EQUIPMENT AND SUPPLIES The following is a list of equipment that may be necessary to carry out the procedures contained in this SOP. Additional equipment may be required. Glove bag or equivalent apparatus Portable nitrogen tank and tubing Core cutting equipment X-ray fluorescence gun Stainless-steel bowls and spoons for processing 2-millimeter (mm) sieve Decontamination equipment Magnesium chloride Sodium acetate Acetic acid Sodium dithionite Sodium citrate Hydrogen citrate Hydroxylamine hydrochloride Nitric acid Hydrogen peroxide Ammonium acetate Centrifuge and tubes Sample agitator/tumbler Sample bottles Sample labels Coolers and ice SAMPLE PREPARATION Select surface and subsurface sample archives will be sequentially extracted at a research facility. Surface samples will arrive to the facility ready for extraction. Subsurface sediments will arrive to the facility in 1-foot sections. An X-ray fluorescence gun will be used to estimate the metals concentration in targeted depths based on Phase 1 total recoverable metals data. After confirmation of selected intervals, the selected 1-foot section of the core Newtown Creek RI/FS

6 will be opened, and the targeted depth will be subsampled, homogenized, and sieved (to obtain a fraction of less than 2 mm). All processing and extraction procedures will be conducted in a positive-pressure nitrogen glove bag, except the agitation and centrifugation steps, which will be in tightly sealed sample tubes. Processed samples will be sequentially extracted using the procedures in the following table. Target Fraction Extraction Fluid Procedure Exchangeable Carbonate bound Reducible iron/manganese oxide bound 1 molar magnesium chloride, ph 7 1 molar sodium acetate, ph 5 with acetic acid 0.3 molar sodium dithionite; molar sodium citrate; molar hydrogen citrate; 0.04 molar hydroxylamine hydrochloride in 25% v/v acetic acid 1. Add 8-mL fluid to 1-gram sample in centrifuge tube. 2. Agitate in tumbler-shaker for 1 hour at room temperature. 3. Centrifuge for 25 minutes at 12,000 grams. 4. Decant fluid. 5. Repeat Steps 1 to 4 with new extraction fluid. 6. Combine all decanted fluid, acidify with HNO 3 to ph <2, and analyze for TAL metals by USEPA 6010/ Repeat Steps 1, 3, and 4 with DI water. 1. Add 8-mL fluid to same 1-gram sample in centrifuge tube. 2. Agitate in tumbler-shaker for 5 hours at room temperature. 3. Centrifuge for 25 minutes at 12,000 grams. 4. Decant fluid. 5. Repeat Steps 1 to 4 with new extraction fluid for 24 hours. 6. Combine all decanted fluid, acidify with HNO 3 to ph <2, and analyze for TAL metals by USEPA 6010/ Repeat Steps 1, 3, and 4 with DI water. 1. Add 20-mL fluid to same 1-gram sample in centrifuge tube. 2. Agitate in tumbler-shaker for 6 hours at room temperature. 3. Centrifuge for 25 minutes at 12,000 grams. 4. Decant fluid. 5. Repeat Steps 1 to 4 with new extraction fluid for 6 hours. 6. Combine all decanted fluid and analyze for TAL metals by USEPA 6010/ Repeat Steps 1, 3, and 4 with DI water. Newtown Creek RI/FS

7 Target Fraction Extraction Fluid Procedure Oxidizable sulfide/organic matter bound 0.02 molar nitric acid, 30% hydrogen peroxide, ph 2; 30% hydrogen peroxide, ph 2 with nitric acid; 3.2 molar ammonium acetate in 20% v/v nitric acid Residual sample USEPA 3050B/6020 Initial sample SM2540G Notes: % = percent DI = deionized HNO 3 = nitric acid ml = milliliter TAL = target analyte list USEPA = U.S. Environmental Protection Agency v/v = volume to volume percent 1. Add 8-, 3-, and 5-mL fluid, respectively, to the same 1-gram sample in centrifuge tube. 2. Agitate in tumbler-shaker for 2, 3, and 0.5 hours, respectively, at room temperature. 3. Centrifuge for 25 minutes at 12,000 grams. 4. Decant fluid. 5. Combine all decanted fluid and analyze for TAL metals by USEPA 6010/ Repeat Steps 1, 3, and 4 with DI water. 1. Send the same 1-gram sample to the analytical laboratory for TAL metals preparation and analysis by USEPA 3050B/6010/ Analyze initial sediment aliquot for total solids (for calculation). SAMPLE HANDLING PROCEDURES Generated samples will be placed in laboratory-provided sample containers and labeled with the project name, sample identification, date and time, and preservative. Samples will then be logged on a chain-of-custody form and sent in a cooler packed with ice to Alpha Analytical Laboratory at the following address: Alpha Analytical Laboratory 320 Forbes Boulevard Mansfield, Massachusetts (508) DATA REDUCTION PROCEDURES Sample preparation volumes, including initial sample weights and extract volumes, should be recorded on chemistry bench sheets. The TAL metal results for extracts will need to be recalculated on the basis of initial sediment sample dry weight using the following calculation: Newtown Creek RI/FS

8 C(sed) [mg/kg] = C(extract) [µg/l] x V(extract) [L] / W(sed) [g dw] SOP AQ-1 where: W(sed) [g dw] = W(sed) [g ww] x (100 MC) C(sed) [mg/kg] = sediment concentration in milligrams per kilogram C(extract) [µg/l] = concentration of the sample extract in micrograms per liter V(extract) [L] = extract volume in liters W(sed) [g dw] = weight of sediment in grams dry weight W(sed) [g ww] = weight of sediment in grams wet weight MC = percent moisture by Method SM2540G QUALITY ASSURANCE/QUALITY CONTROL It is the responsibility of the risk assessment task leads to periodically check to ensure that the procedures are in conformance with those stated in this SOP. REFERENCES Anchor QEA (Anchor QEA, LLC), Environmental Geochemistry Laboratory Chemical Hygiene Plan. Version 1.0. February 1, Anchor QEA, 2014a. Phase 2 Remedial Investigation Work Plan Volume 1. Draft. Remedial Investigation/Feasibility Study, Newtown Creek. April Anchor QEA, 2014b. Phase 2 Quality Assurance Project Plan. Draft Appendix A of the Phase 2 Remedial Investigation Work Plan Volume 1. Remedial Investigation/Feasibility Study, Newtown Creek. April Anchor QEA, 2013c. Phase 2 Field Sampling and Analysis Plan Volume 1. Draft Appendix B to the Phase 2 Remedial Investigation Work Plan Volume 1. Remedial Investigation/Feasibility Study, Newtown Creek. April Tessier et al. (Tessier, A., P.G.C. Campbell, and M. Bisson), Sequential Extraction Procedure for the speciation of Particulate Trace Metals. Analytical chemistry 51(7): Newtown Creek RI/FS

9 Zimmerman and Weindorf (Zimmerman, A.J. and D.C. Weindorf, Heavy Metal and Trace Metal Analysis in Soil by Sequential Extraction: A Review of Procedures. International Journal of Analytical Chemistry Newtown Creek RI/FS