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. ? ?AMENDMENT 2

(October 1995)

to the

Sediment/Soil Investigation Studies

Mississippi River Pool 15

Phase HI Field Sampling Plan

of July 1995

This document provides a revised mussel sampling strategy representing a modification to the

Sediment/Soil Investigation Studies, Mississippi River Pool 15, Phase III Field Sampling Plan

dated July 1995. Following approval by EPA, this amendment shall be incorporated into, and be

adhered to as part of the Phase HI Field Sampling Plan.

The objectives of the mussel survey are to:

• .identify the presence of unionid mussels on the Federal Endangered Species List,

specifically Lampsilis higginsi; and

• determine the current status (species composition and density) of any mussel beds

and habitat that may exist within the study area.

• characterize PCB contamination in mussels adjacent to the Alcoa Facility.

The revised strategy for meeting these objectives will be based on a stratified random sampling

approach using diving to collect mussels. Quantitative sampling will be accomplished by collecting

unionids within 0.5 m x 0.5 m (0.25 m2) quadrats at 20 randomly selected locations along a 160-m

(about 500-ft) transect. Transects will be positioned perpendicular to shore and will be spaced

approximately 500 ft (or less) apart along Critical Study Areas 1A, IB and 1C. A 160-m weighted

rope marked with chains at 25-ft intervals will be used to mark the transect for the divers. Twenty

random sampling locations along the transect will be selected from a random numbers table to

identify sampling locations. Sampling locations that fall between the marked 25-ft intervals will be

estimated by the diver. Divers will collect all unionids within the 0.25-m2 quadrat at each

Amendment 2Sediment/Soil Investigation Studies of2

randomly-selected location and place them in a mesh bag. The mussels from each bagged sample

will be identified, measured and counted in order to determine species diversity and density (tf/m2)

by a trained malacologist. Mussel ages will be estimated in the field. All sampling will be

conducted in accordance with the conditions stipulated in Federal Fish and Wildlife Permit Number

PRT 805737.

If sufficient mussels are located, up to 12 mussel samples will be collected for PCB analyses from

Area 1 A, IB, and 1C (for example, 4 samples from each CSA) and 5 samples from Reference Area

1. These samples will be submitted for analysis of PCBs. All remaining mussels will be released

near the location from which they were collected. Surface sediment (0-0.5 ft) will be sampled at

locations where mussels are collected for tissue analyses using methods outlined in the FSP. The

sediment samples will be analyzed for PCBs, TOC and particle size.

The species collected for tissue analyses will be decided in the field based on availability. An

attempt will be made to collect mussels of similar size for analysis both within and between

sampling locations. These mussels will be measured, aged and soft tissue removed. Tissue

samples will be placed in precleaned jars, iced and shipped under chain-of-custody to the analytical

laboratory. Sediment samples will be containerized and submitted for analysis in accordance with

in the FSP.

GREGORY E. THOMAS laboratory directorsoils testingseismic studies

EDUCATION

Rensselaer Polytechnic Institute: M.E., Geotechnical Engineering, 1979Rensselaer Polytechnic Institute: B.S., Civil Engineering, 1977Rensselaer Polytechnic Institute: B.S., Geology, 1977

PROFESSIONAL HISTORY

Woodward-Clyde Consultants, Laboratory Director, 1994 to dateGEI Consultants, Inc., Laboratory Director, Geotechnical Engineering Division, 1989- 1994ISMES, S.pA, Bergamo, Italy, Project and Research Engineer, Geotechnical Laboratory

Department, 1984-1989Rensselaer Polytechnic Institute, Department of Civil Engineering, Laboratory Assistant,

1982; StaffEngineer, 1982-1984

REPRESENTATIVE EXPERIENCE

As Director of Woodward-Clyde's Totowa, NJ Geotechnical Laboratory, Mr. Thomas' primaryresponsibility is the management of the laboratory which includes the development andimplementation of a quality control program, and the direction of a state-of-the-art geotechnicalsoils testing facility. His duties include the supervision of laboratory personnel and testingprograms and the development and application of advanced laboratory testing techniques.

Mr. Thomas is a member of ASTM Committee D18 on soil and rock and is currently active onsubcommittees on the structural, cyclic and dynamic properties of soil.

Specific soils laboratory experience includes:

• Supervision of the development and implementation of a computerized data acquisitionsystem - allowing real time analysis of tests using a spreadsheet environment.

• Extensive experience in laboratory testing for nuclear power industries in Italy and Pakistan.Served as project coordinator and laboratory advisor on nuclear site investigations.

• Involved in numerous investigations concerning the seismic analysis of earth and tailingdams.

• Involved in numerous projects concerning bearing capacity evaluation, slope stabilityassessment and landfill liner material acceptability.

gd95.doc

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GREGORY E. THOMAS page2

Specific project experience includes:

• Central Artery (1-93)/funnel (1-90) Project, Boston, Massachusetts - Directed the laboratory test program for the Central Area geotechnical study. Testing included classification, consolidation, penneability, static and cyclic shear tests, and Ko consolidated oompression and extension triaxial tests on soils.

• Clemson Upper and Lower Diversion Dams, Clemson, South Carolina - Directed the laboratory test program for the seismic evaluation of the dams. Testing included conventional and steady state tests.

• Pakistan Atomic Energy Commission, Chasma Site, Pakistan - Directed dynamic laboratory investigation concerning liquefaction assessment for potential sites for nuclear power plant. Test included cyclic triaxial, cyclic simple shear, resonant column tests and associated classification and static tests.

• ENEL, Po 2 Site, Milan, Italy - Project coordinator for the laboratory investigation for a proposed nuclear power plant site. Investigation included complete static and dynamic testing programs for the determination of bearing capacity, settlement, cyclic settlement, and cyclic stability of the site.

• SOILCON, Lahore, Pakistan - Advised and assisted in the development of the Pakistan Atomic Energy Commission geotechnical and material testing laboratory.

• Landfill Liner Acceptability Tests, Various Sites in Massachusetts - Directed laboratory testing to verify t~e suitability of construction materials in terms of soil classification,·· compaction and permeability requirements.

Prior to joining Woodward-Clyde, Mr. Thomas was Laboratory Director of the Geotechnical Engineering Division of GEi Consultants, Inc. where he was responsible for the training, supervision and scheduling of laboratory staff, the development and modification of laboratory procedures, and equipment maintenance.

AFFILIATIONS

American Society for Testing and Materials American Society of Civil Engineers

015090lt001. TOT.9194

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GREGORY E. THOMAS page3

PUBLICATIONS

A re-evaluation of conventional triaxial test methods (with G. Baldi and D.W. Hight). Advanced ' Triaxial Testing of Soil and Rock. American Society of Testing and Materials. Philadelphia.

STP 977, 1988.

Cyclic simple shear strain-controlled behavior of one overconsolidated offshore clay (with M. Vucetic, R Dobry, and E. Petrakis). Proceedings Section International Conference on Soil Dynamics and Earthquake Engineering. Vol. 2, pp. 107-116, 1985.

Influence of consolidation shear stresses and relative density on threshold strain and pore pressure during cyclic straining of saturated sand (with R Dyvik, R Dobry and W.G. Pierce). U.S. Army Corps ofEngineers. Miscellaneous paper GL-84-15, 1985.

Cyclic strain-controlled tests for liquefaction studies of saturated debris from Mount St. Helen volcanic explosion (with R Dobry). RPI Civil Engineering Report No. CE-84-4 to

the U.S. Geological Survey. 1984.

Study of Venezuelan marine soils: phase 1 static and cyclic testing and characterization of offshore tuy cariaco clay (with M. Vucetic and R ·Dobry). RPI Civil Engineering Report to Institute Technologico Venezolano del Petroleo, Los Teques, Venezuela, 1982.

Experimental study of the cyclic constitutive relation of saturated sands during undrained loading- equipment development and preliminary results (with R Dyvik, R Dobry and RS.

Ladd). RPI Civil Engineering Report No. CE-82-1 for the National Science Foundation, 1982.

Equivalent spring and damping coefficients for piles subjected to vertical dynamic loads. Masters Project, Rensselaer Polytechnic Institute, Troy, New York, 1977.

01 S090ROOI. TOT.9194

Geotechnical Laboratory Services

Woodward-Clyde can provide you with conventional and state-of-the-art geoteclmical laboratory testing for all of your design or construction needs. We offer current technology, diverse staff expertise, strict quality control, accessible project teams, and a thorough knowledge of testing standards. Our largest laboratory - in Totowa, N.J. - is among the best and most sophisticated in the world.

Client Needs You need a complete geoteclznical laboratory service, providing planning, perfonnance, property characterization, and reports for a broad spectrum of laboratory tests.

In today's competitive market, innovative and economical solutions are essential. The use of general assumptions on material and site characteristics leads to solutions that may not be cost effective or may lead to a disappointing performance. As a result, successful design and construction professionals are using strategic laboratory testing to obtain the solution that best meets project requirements. To do that, you need a laboratory that does the following: • Implements the latest in geotechnical

testing methodology • Offers testing solutions within your

project schedule and budget • Provides a local representative

available to help you • Offers consistent staff and services

throughout the project • Offers flexibility and innovation in

laboratory testing • Understands testing programs that

promote cost effectiveness • Understands testing standards and

regulatory requirements • Sweats the testing details for you

LABORATORY SERVICES • ~ ~

Client Benefits

Woodward-Clyde has successfully completed thousands of testing programs for a wide range of projects. We are confident our service makes us stand out from other laboratories.

We give vou a commitment to qµalit,y laboratory testing that leads to successfu.l project comoletion.

We have been in the testing business for over 40 years. We train our staff rigorously on standard procedures. We calibrate our equipment regularly and review all test results. We offer knowledgeable flexibility on test procedures and data presentation to accommodate each client's needs .

Our experience can help vou develoo a quality testing proeram with competitive pricing.

We will work with you to develop a testing program tailored to your project requirements , financial needs, and schedule. Our experience has given us an in-depth understanding of the construction process that helps us to accurately estimate costs and schedules.

Our company structure offers you regional laboratories.

We have 13 U.S. laboratories to serve your local needs. For specialized testing or large testing programs, local personnel can coordinate testing at our larger laboratories.

Our ability to channel workloads provides timely response.

Through our U.S.-wide network, we have the equipment and testing personnel to provide fast tum-around times to meet your deadlines.

We have the unique abilit,y to test contaminated materials.

Our New Jersey laboratory is one of only a few geotechnical laboratories capable of testing contamillated materials following all Federal Rules and Regulations for personal safety and material handling.

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Experience

Over the years, our clients have challenged us with many geotechnical testing problems. Some examples are:

• Confidential Site A soil-bentonite mix was needed for use in a cutoff wall in a contaminated environment. We worked with the contractor to develop an innovative design mix suited to the contractor's equipment and construction methods. We tested the mix using site-specific leachate lo demonstrate its resistance to degradation. Field testing performed after installation of the wall provided field test results agreeing with those from design tests.

• Domenigoni Valley Dam -California We employed a U.S.-wide approach to provide the diverse laboratory services required for investigating, analyzing, and designing two 84-million-yd3 dams. This required using a field laboratory for tests requiring rapid results and testing throughout Woodward-Clyde's laboratories to satisfy the complete scope of testing in a timely and economic manner. The program included index, permeability, drained and undrained triaxial strength, cyclic strength and property triaxial, cyclic strength direct simple shear, and resonant column tests .

• Kennecott - Utah As part of the design for the expansion of the largest tailings dam in the world, we performed a comprehensive test program on the soft foundation sediments and tailings materials . Testing included state-of-the-art static and cyclic triaxial and direct simple shear strength tests on undisturbed and special slurry sedimented tailings samples . Testing provided normalized stress parameters used in critical design nonlinear dynamic deformation analyses.

Services

We provide services for testing programs from one sample to hundreds of samples. We test samples for foundations, dams and highway embankments, landfill caps and liners, soil-bentonite, cement-bentonite and plastic concrete slurry walls, waste management, and a variety of soil admixtures. Standard testing services offered follow ASJ'M test methods. COE, EPA, ISRM, AASHTO, and state-of-the-art methods are also routinely pelfonned. The extensive soil and rock testing capabilities include:

• Index and physical properties testing • Compaction testing • Consolidation testing • Permeability and compatibility testing • Strength testing • Cyclic strength and properties testing • Slurry wall mix design testing • RCC mix design testing • Contaminated materials testing • Special parameters testing

Laboratory Locations Woodward-Clyde has laboratories in

Totowa, NJ, Pleasant Hill, CA, San Diego, CA, Santa Ana, CA, Denver, CO, Overland Park, KS, Baton Rouge, LA, Gaithersburg, MD, St. Louis, MO, Omaha, NE, Cleveland, OH, Philadelphia, PA, and Milwaukee, WI.

Woodward-Clyde Facts

• Founded in 1950 • More than 85 offices and over 2 ,800

employees worldwide • Performs planning, consulting,

permitting, design, construction, and operations

• For more information on our ability to help you with services involving geotechnical laboratory testing, contact Greg Thomas in New Jersey at (201) 812-1818, Sam Capps in California at (510) 746-6650, or by Email at [email protected].

LAB DOC 1995

.,

Geotechnical Laboratory Services (Totowa, NJ)

Why should you choose WoodwardClyde's Geotechnica1 Laboratory?

We are confident our service makes us stand out from other laboratories. You, our client, will receive:

• Quality laboratory testing. We have been in the testing business for over 40 years. We train our staff rigorously to follow standard procedures. Our equipment is calibrated frequent! y and all test results are reviewed.

• Timely response. We have the equipment and testing personnel to provide fast-turnaround times, and above all, your deadlines are sacred for us and we will meet them.

• Competitive pricing. We will work with you to develop an economical testing program tailored to your financial needs, not our needs.

For More Infonnation

To put the Woodward-Clyde geotechnical laboratory to work for you, please contact Greg Thomas or Carolynn Tobin at:

Phone: Fax: E-mail

(201) 812-1818. (201) 812-8640 [email protected]

Woodward-Clyde Consultants Geotechnical Testing Facility 45H Commerce Way Totowa, NJ 07512

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geotechnical laboratory takes on your testing projects, we make a strong commitment to you, our client, to provide you with quality testing in a timely man..ner. We respond to your needs, not ours, and make sure that you receive real value for your money.

Testing is performed in a modern 10,000 square foot, temperature-controlled facility. This facility, equipped with up to date instrumentation, is largely automated and operates under strict quality assurance procedures. The facility contains a hum.id room for specimen preparation and undisturbed sample storage as well as a large section devoted to the testing of contaminated materials. All the necessary equipment and full-time personnel are available to perform several major testing programs simultaneously. Testing procedures, including data collection, reduction and presentation, are flexible to accommodate each client's needs.

This facility is one of the most advanced commercial geotechnical laboratories in the country. It is a leader in the fields of hydrogeologic properties of soils and soil liners; normalized behavior of soil and soft rock; and cyclic testing for earthquake and offshore wave analysis.

Additionally, our laboratory is one of only a few geotechnical laboratories capable of testing contaminated materials following all Federal Rules and Regulations for personal safety and material handling.

Controlled QQWX^m,.__,_.ronvNo UNCONTROLLED COPYCopy No.

SOP No. NC-OP-OQQ2Revision No. Q.Revision Date: 10/11/95Page 1 of35

QUANTERRA STANDARD OPERATING PROCEDURE

TITLE: SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION METHOD 3510 FORBNA/PAH 625/8270 PESTICIDES/PCBS 608/8080 TPH BY GC. OPP 8141. 9100. PAH'S 8310

(SUPERSEDES: ENSECO SOP #LM-WALN-5010 (DRAFT))

Prepared by:

Reviewed by:

Approved by:

Approved by:

Approved by:

Technology Specialist

Quality Assurance

Environmental Health and Safety Coordinator

Laboratory Director

Proprietary Information Statement:

This document has been prepared by and remains the sole property of Quanterra Incorporated. It issubmitted to a client or government agency solely for its use in evaluating Quanterra's qualifications inconnection with the particular project, certification, or approval for which it was prepared and is to beheld propriety to Quanterra.

The user agrees by its acceptance or use of this document to return it upon Quanterra's request and not toreproduce, copy, lend, or otherwise disclose or dispose of the contents, directly or indirectly, and not touse it for any propose other than that for which it was specifically furnished. The user also agrees thatwhere consultants or others outside of the user's organization are involved in the evaluation process,access to these documents shall not be given to those parties unless those parties also specifically agreeto these conditions.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. £608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_lfi/U/25_

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TABLE OF CONTENTS

1. SCOPE AND APPLICATION ., 3

2. SUMMARY OF METHOD 3

3. DEFINITIONS 3

4. INTERFERENCES 3

5. SAFETY 3

6. EQUIPMENT AND SUPPLIES ....4

7. REAGENTS AND STANDARDS 5

8. SAMPLE COLLECTION, PRESENTATION AND STORAGE. 6

9. QUALITY CONTROL 6

10. CALIBRATION AND STANDARDIZATION 8

21. PROCEDURE 8

12. DATA ANALYSIS AND CALCULATIONS...... 13

13. METHOD PERFORMANCE 13

14. POLLUTIONPREVENTION. 14

15. WASTE MANAGEMENT. 14

16. REFERENCES 14

17. MISCELLANEOUS (TABLES, APPENDICES, ETC...) 15

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0.608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_lMl/25

Page 3 of35

1. SCOPE AND APPLICATION

1.1. This SOP, based on SW846 Method 351OA and EPA Method 600/4-81 -045, describes aprocedure for isolating organic compounds from aqueous samples. The method alsodescribes concentration techniques suitable for preparing the extract for the appropriatedeterminative methods.

1.2. This method is applicable to the isolation and concentration of water-insoluble andslightly water-soluble organics in preparation for a variety of chromatographicprocedures.

1.3. This document accurately reflects current laboratory standard operating procedures (SOP)as of the date above. All facility SOPs are maintained and updated as necessary by thelaboratory QA department.

2. SUMMARY OF METHOD

2.1. A measured volume of sample is placed into a separatory funnel extractor, adjusted, ifnecessary, to a specified pH, and extracted with organic solvent for 3 sets of 1-2 minuteshakes. The extract is dried, concentrated, and as necessary, exchanges into a solventcompatible with the cleanup or determinative step to be used.

3. DEFINITIONS

3.1. Refer to the glossary hi the Quality Assurance Management Plan (QAMP).

4. INTERFERENCES

4.1. Method interferences may be caused by contaminants in solvents, reagents, glassware,and other processing apparatus that lead to discrete artifacts. All of these materials mustbe routinely demonstrated to be free from interferences under conditions of the analysisby running laboratory method blanks as described in the Quality Control section.Specific selection of reagents may be required to avoid introduction of contaminants.

5. SAFETY

5.1. Procedures shall be carried out in a manner that protects the health and safety of allQuanterra associates.

5.2. Eye protection that satisfies ANSI Z87.1 (as per the Chemical Hygiene Plan), laboratorycoat, and appropriate gloves must be worn while samples, standards, solvents, and

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 4 of35

reagents are being handled. Disposable gloves that have been contaminated will beremoved and discarded; other gloves will be cleaned immediately.

i

5.3. The health and safety hazards of many of the chemicals used in this procedure have notbeen folly defined. Additional health and safety information can be obtained from theMaterial Safety Data Sheets (MSDS) maintained in the laboratory. The followingspecific hazards are known:

5.3.1. Chemicals that have been classified as carcinogens, or potential carcinogens,under OSHA include: Methylene Chloride.

5.3.2. Chemicals known to be flammable are: Hexane, Acetone.

5.3.3. The following materials are known to be corrosive: Sulfuric Acid, SodiumHyroxide.

5.4. Exposure to chemicals must be maintained as low as reasonably achievable, therefore,unless they are known to be non-hazardous, all samples must be opened, transferred andprepared in a fume hood, or under other means of mechanical ventilation. Solvent andwaste containers will be kept closed unless transfers are being made.

5.5. The preparation of standards and reagents will be conducted hi a fume hood with thesash closed as far as the operation will permit. x

5.6. All work must be stopped in the event of a known or potential compromise to the healthand safety of a Quanterra associate. The situation must be reported immediately to alaboratory supervisor.

6. EQUIPMENT AND SUPPLIES

6.1. Separatory funnel: 2-liter, with Teflon® stopcock

6.2. Pyrex glass funnel, 75 x 75 mm

6.3. Kuderna-Danish (K-D) apparatus

6.3.1. Concentrator tube: 10 mL, graduated (Kontes K-570050-1025 or equivalent).Ground-glass stopper is used to prevent evaporation of extracts.

6.3.2. Kuderna-Danish: 500 mL (Kontes K-570001-500 or equivalent). Attach toconcentrator tube with clips.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_lMl/25_

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6.3.3. Snyder column: Three-ball macro (Kontes K-503000-0121 or equivalent)

6.3.4. Snyder column: Two-ball micro (Kontes K-569001-0219 or equivalent)

6.4. Boiling chips: Solvent extracted, approximately 10/40 mesh (silicon carbide orequivalent) .

6.5. Water bath: Heated, with concentric ring cover, capable of temperature control (±5°C).The bath should be used in a hood.

6.6. Vials: Glass, 2 mL and 10 mL capacity with Teflon®-lined screw-cap

6.7. pH indicator paper: pH range including the desired extraction pH

6.8. Erlenmeyer flask: 250 mL

6.9. Syringe: 1 mL

6.10. Graduated cylinder: 1 liter

6.11. Glass wool

6.12. Organomation N-EVAP Model 112 or equivalent

7. REAGENTS AND STANDARDS

7.1. Reagents

7.1.1. Sodium Hydroxide NaOH, Pellets: Reagent Grade

7.1.2. Sodium Hydroxide Solution, 1 ON: Dissolve 40 g of NaOH in reagent water anddilute to 100 mL.

7.1.3. Sodium Sulfate (Na2S04), Granular, Anydrous: Purify by heating at 400°C aminimum of four hours.

7.1.4. Sulfuric acid (H2SO4), Concentrated: Reagent Grade

7.1.5. Sulfuric Acid (1:1): Carefully add 500 mL of H2S04 to 500 mL of reagent water.Mix well.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. &608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_MH/9_5_

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7.1.6. Extraction/Exchange Solvent: Methylene chloride, hexane, acetonitrile, pesticidequality or equivalent.

7.2. Acetone-Used to clean syringes

7.3. Reagent Water

7.4. Standards-See Appendix I

8. SAMPLE COLLECTION, PRESERVATION AND STORAGE

8.1. Samples are not chemically preserved.

8.2. Samples are stored at 4°C ± 2°C in glass containers with Teflon®-lined caps.

8.3. Extraction is initiated within seven days of the sampling date.

8.4. For TCLP leachates, extraction is initiated within seven days from when the leachingprocedure is initiated.

8.5. Analysis of the extracts is completed within forty days of extraction.

9. QUALITY CONTROL

9.1. Batch Definition

9.1.1. A batch is a group of no greater than 20 samples excluding QC samples (LCS,Method Blank, MS, MSD) which are processed similarly, with respect to theprocedure. All sample setups must be initiated within a 24 hour period from theinitial preparation or extraction and without interruption of the process. Allsamples within the batch must be treated with the same lots of reagents and thesame processes.

9.2. Method Blank

9.2.1. One method blank (MB) must be processed with each preparation batch. Themethod blank consists of reagent water containing all reagents specific to themethod that is carried through the entire analytical procedure, includingpreparation and analysis. The method blank is used to identify any system andprocess interferences or contamination of the analytical system that may lead tothe reporting of elevated analyte concentrations or false positive data. The

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

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method blank should not contain any analyte of interest at or above the reportinglimit.

9.3. Laboratory Control Sample (LCS)

9.3.1. One aqueous LCS must be processed with each preparation batch. The LCS mustbe carried through the entire analytical procedure. The LCS is used to monitor theaccuracy of the analytical process. On-going monitoring of the LCS resultsprovides evidence that the laboratory is performing the method within acceptableaccuracy and precision guidelines.

9.3.2. Table 7 indicates the volume and type of LCS spiking solution to be used in eachtype of extraction.

9.4. Matrix Spike/Matrix Spike Duplicate (MS/MSD)

9.4.1. One MS/MSD pair must be processed for each batch. A matrix spike (MS) is afield sample to which known concentrations of target analytes have been added.A matrix spike duplicate (MSD) is a second aliquot of the same sample (spikedidentically as the MS) prepared and analyzed along with the sample and matrixspike. Some client specific data quality objectives (DQO's) may require the useof sample duplicates in place of or in addition to MS/MSD's. The MS/MSDresults are used to determine the effect of a matrix on the precision and accuracyof the analytical process. Due to the potential variability of the matrix of eachsample, these results may have immediate bearing only on the specific samplespiked. Samples identified as field blanks cannot be used for MS/MSD analysis.

9.4.2. Table 9 indicates the volume and type of matrix spiking solution to be used ineach type of extraction.

9.5. Surrogates

9.5.1. Surrogates are organic compounds which are similar to the target analyte(s) inchemical composition and behavior in the analytical process, but which are notnormally found in environmental samples.

9.5.2. Each sample, blank, and MS/MSD is spiked with surrogate standards. Surrogatespike recoveries must be evaluated by determining whether the concentration(measured as percent recovery) falls within the required recovery limits.

9.5.3. Add 1 mL of surrogate compounds to each sample.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_MLl/9_5_

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9.5.4. Table 8 indicates the volume and type of surrogate spiking solution to be used ineach type of extraction.

10. CALIBRATION AND STANDARDIZATION

10.1. Not Applicable

11. PROCEDURE

11.1. One time procedural variations are allowed only if deemed necessary in the professionaljudgment of supervision to accommodate variation in sample matrix, radioactivity,chemistry, sample size, or other parameters. Any variation in procedure shall becompletely documented using a Nonconformance Memo and is approved by a TechnicalSpecialist and QA Manager. If contractually required, the client shall be notified. TheNonconformance Memo shall be filed in the project file.

11.2. Any unauthorized deviations from this procedure must also be documented as anonconformance, with a cause and corrective action described.

11.3. Sample Preparation Summary

11.3.1. A measured volume of sample, usually 1 liter, at a specified pH (see Table 5), isserially extracted with methylene chloride using a separatory funnel. The extractis dried, concentrated, and, as necessary, exchanged into a solvent compatiblewith the cleanup or determinative step to be used. : " .: .

11.4. Sample Preparation Procedure

11.4.1. With the exception of TCLP samples, mark the meniscus level on the sample jar.Transfer the sample to the separatory funnel. Less than one liter of sample maybe used and diluted to 1 liter with fresh reagent water. All containers must berinsed (if entire container is used) with solvent or reagent water to removeresidual analyte adhering to glass walls and added to the separatory funnel. Fillthe sample jar with water up to the marked level. Transfer the measured amountof water to a graduated cylinder and record the volume on the benchsheet to thenearest 5 mL mark.

11.4.2. Add 1.0 mL of the surrogate standards to all samples, spikes, and blanks and mixwell, (see Section 9 for details on the surrogate standard solution and the matrixspike solution). For the sample in each analytical batch selected for spiking, add1.0 mL of the matrix spiking standard.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTIONMETHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310

SOP No. NC-OP-0002Revision No. QRevision Date: 10/11/95Page 9 of 35

Water Sample

Solvent

Stop

Figure 1 Separatory Funnel

11.4.3. Check the pH of the sample with a wide-range pH paper and, if necessary, adjustthe pH to that indicated in Table 5 for the specific determinative method that willbe used to analyze the extract. Mix well before measuring pH. Record the pH.NOTE: Double check the pH of all buffered samples (e.g. TCLP).

11.4.4. Add 60 mL of methylene chloride to the separatory funnel.

11.4.5. Seal and shake the separatory runnel vigorously for 2 minutes with periodicventing to release excess pressure.

WARNING: Methylene chloride creates excessive pressure very rapidly! Therefore,initial venting should be done immediately after the separatory funnel hasbeen sealed. Vent into hood away from other samples.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:_lim/9_5_

11.4.6. Allow the organic layer to separate from the water phase for a minimum of 10minutes. If the emulsion interface between layers is more than one-third the sizeof the solvent layer, the analyst must employ mechanical techniques to completethe phase separation. The optimum technique depends upon the sample and mayinclude stirring, filtration of the emulsion through glass wool, centrifugation, orother physical methods. If the emulsion cannot be broken (recovery of <80% ofthe methylene chloride, transfer the sample, solvent, and emulsion into theextraction chamber of a continuous extractor and proceed as described in Method3520.

11.4.7. Assemble a Kuderna-Danish (K-D) concentrator apparatus by attaching a 10 mLconcentrator tube to a 500 mL K-D evaporation flask. Attach a clamp to theflask/concentrator tube Joint (see Figure 2). If K-D is not available another glasscontainer is appropriate (ie., Erylemeyer or Beaker).

11.4.8. Prepare a funnel with a small amount of glass wool as a plug and pourapproximately 40 g of anhydrous sodium sulfate into the funnel. Place theprepared funnel into the ground glass joint at the top of the K-D apparatus.Prerinse as needed the filter and K-D apparatus with solvent and discard.

11.4.9. Dram the methylene chloride extract layer through the funnel into the K-D. Closethe stopcock just before the water level drains into the funnel.

11.4.10.Repeatthe extraction two more times using fresh portions of solvent.. Combinethe three solvent extracts.

11.4.11.If further pH adjustment and extraction is required, adjust the pH of the aqueousphase to the desired pH indicated in Table 1. Serially extract three more timeswith 60 mL of methylene chloride, as outlined in Steps 11.2.3 through 11.2.3.Collect and combine the extracts and label the combined extract appropriately.

11.4.12.1f performing GC/MS analysis (Method 8270), the acid and base/neutral extractsmay be kept separate or be combined.

11.4.13.Rinse the sodium sulfate in the funnel by pouring 20-30 mL of clean methylenechloride through the funnel and into the K-D.

11.4.14.Pre-wet the three-ball Snyder column by rinsing the Methylene chloride, anddiscarding the Methylene chloride in the appropriate waste container. Add one ortwo clean boiling chips to the flask and attach a three-ball Snyder column to thetop of the evaporating flask. Place the K-D apparatus on a hot water bath, 80° -90° C, so that the concentrator tube (CT) is partially emersed in the hot water and

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 11 of 35

the entire lower rounded surface of the flask is bathed with hot vapor. At theproper rate of distillation, the balls of the column will actively chatter, but thechambers will not flood. Continue the concentration procedure until the apparentvolume of liquid in the CT approaches the final extract volume. Caution: Theconcentrated volume must be near but above the final volume. If the extract doesnot require a solvent exchange, remove the K-D apparatus from the water bath.Allow it to drain and cool for at least ten minutes and remove the Snyder column.Proceed to Section 11.6.4. If a solvent exchange is required continue with Section11.63.1.

11.4.14.1.If the determinative method is for Pesticides and/or PCBs, a solventexchange with hexane is required. When the apparent volume of theliquid in the CT approaches 2 mL, add approximately 50 ML of hexane tothe Snyder column.

11.4.14.2.Concentrate the extract, as described in 11.6.3, raising the temperatureof the water bath, if necessary, to maintain proper distillation. Caution:The concentrated volume must be near but above the final volume. Allowthe solvent to drain as it cools and remove the Snyder column. Proceed toSection 11.6.4.

11.4.15.Since extracts analyzed for Pesticide/PCBs and/or PAHs require larger finalvolume (5 mL), the extracts must be transferred to centrifuge tubes for accuratevolume measurement. Remove the concentrator tube and transfer the extract to acalibrated centrifuge tube. Rinse the concentrator tube with the appropriatesolvent, adding the rinse to the centrifuge tube. Extracts requiring 1.0 mL finalvolume remain in the CTs. Place the extract on the nitrogen blowdown apparatus.Adjust the temperature of the nitrogen blowdown water bath to 35°C.

11.4.16.Evaporate the extract using a gentle stream of clean, dry nitrogen to just belowthe final extract volume for analysis as indicated hi Table 1. Recommended flowrate is 3-4 mL/min. The extract must never be allowed to go dry.

11.4.16.1.To prevent phthalate and cross-contamination between samples, thetubing delivering the nitrogen must never come in contact with the extract.If they do come in contact with the extract, the tubing must be thoroughlycleaned with the solvent.

11.4.17.During evaporation, the solvent level in the centrifuge tube or CTs must be keptbelow the water level of the bath. The top of the centrifuge tube or CT must bepositioned above the water line to avoid water condensation in the extract.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTIONMETHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PGBS608/8080 TPH BY GC OPP 8141 PAHS 8100,8310

SOP No. NC-OP-0002Revision No. 0_Revision Date: 10/11/95Page 12 of 35

Macro Snyder

•250 ml Flask

-Clip

10 ml Receiver

Figure 2 Kudema-Danish Concentrator

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-QQQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 13 of 35

11.4.18.Bring the extract up to the final volume by rinsing the internal wall of thecentrifuge tube of CTs with the appropriate solvent.

11.4.19.Transfer the extract to labeled glass vials. Tightly cap the vial. Double checklabels to ensure all pertinent information is present. Document any anomalies onthe benchsheet. Deliver bottled extracts, with benchsheets and any additionalpaperwork to the analytical group once data has been reviewed.

11.5. Sample Cleanup Procedures

11.5.1. Cleanups hi Table 6 may be applicable. Check the specifics hi each particularcleanup method.

11.6. Sample Analysis

11.6.1. Not Applicable

11.7. Analytical Documentation

11.7.1. Record all analytical information in the analytical logbook/logsheet, including theanalytical data from standards, blanks, LCSs, MS/MSDs, and any correctiveactions or modifications to the method.

11.7.2. All standards are logged into a department standard logbook. All standards areassigned a unique number for identification. Logbooks are reviewed by thesupervisor or designee.

11.7.3. Documentation such as all associated instrument printouts (final runs, screens,reruns, QC samples, etc.) and daily calibration data corresponding to all final runsis available for each data file.

11.7.4. Sample results and associated QC are entered into the LIMs after final technicalreview.

12. DATA ANALYSIS AND CALCULATIONS

12.1. Not Applicable

13. METHOD PERFORMANCE

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-QQQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date:JMlZ25.

Page I±ol3_5_

13.1. Each laboratory must have initial demonstration of performance data on file andcorresponding method detection limit files.

13.2. Training Qualifications:

13.2.1. The group/team leader has the responsibility to ensure that this procedure isperformed by an associate who has been properly trained in its use and has therequired experience.

14. POLLUTION PREVENTION

14.1. This method does not contain any specific modifications that serve to minimize orprevent pollution.

15. WASTE MANAGEMENT

15.1. Methylene chloride saturated water is transferred to the solvent waste cans.

15.2. Solvent waste is disposed of in the red solvent waste cans.

15.3. Acid waste must be collected hi clearly labeled acid waste containers.

15.4. Solid materials (gloves, soiled paper products, etc.) are placed hi the solid debriscontainer. Do not put liquids hi the solid waste container.

15.5. Refer to the Laboratory Sample and Waste Disposal plan.

15.6. Laboratory personnel assigned to perform hazardous waste disposal procedures musthave a working knowledge of the established procedures and practices of Quanterra.They must have training on the hazardous waste disposal practices upon initialassignment to these tasks, followed by an annual refresher training.

16. REFERENCES

16.1. References

16.1.1. SW846, Test Methods for Evaluating Solid Waste, Third Edition, Method 3510A.

16.1.2. EPA 600, Methods for Chemical Analysis of Water and Wastes, Method 600/4-81-045

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 15 of 35

16.2. Associated SOPs

16.2.1. Continuous Liquid/Liquid Extraction Method 3520 for BNA/PAH 625/8270,Pesticides/PCBs 608/8080, TPH by GC, LM-WALN-5020

16.2.2. GC/MS Semivolatile Organic Compounds Base/Neutrals and Acids Method 625,LM-WALN-3030

16.2.3. GC/MS Semivolatile Organic Compounds Capillary Column Technique Method8270, NC-MS-0004.

16.2.4. Pesticides/Polychlorinated Biphenyls by Method 608, LM-WALN-4050

16.2.5. Pesticides/Polychlorinated Biphenyls by Method 8080, LM-WALN-4060

16.2.6. Total Petroleum Hydrocarbons by Gas Chromatography, NC-GC-0013

17. MISCELLANEOUS (TABLES, APPENDICES, ETC...)

17.1. Reporting limits (RL)

17.1.1. Refer to the individual methods listed in Table 5 for specific analyte reportinglimits.

17.1.2. If samples require dilution or smaller volumes than specified in this method, theRL will be elevated.

17.2. Troubleshooting guide

17.2.1. Watch for excessive leaking around the stopper at the top of the separatory funnelduring shaking.

17.2.2. Tighten the stopcock to prevent leaking.

17.2.3. Caution must be taken to keep water out of the extract.

17.2.4. Avoid contamination by keeping gloved hands away from flow of extract whenopening stopcock.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 16 of 35

SURROGATE STANDARD STOCK SOLUTIONPREPARATION


SOP No. NC-OP-Q002Revision No. 0_Revision Date: 10/11/95Page 17 of 35

Table 1 Surrogate Standard Stock Solution Preparation

Type

BNA

Pest/PCB

Pest/PCB

Compound

2-Flurorbiphenyl

2-Fluorophenol

Nitrobenzene-d5

Phenol-d6

p-Terplhenyl-d14

2,4,6-Tribromophenol

Dibutylchlorendate

Tetrachloro-m-xylene

Solvent

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Acetone

Acetone

Neat Mass

(g)

1.0

2.0

1.0

1.0

1.0

2.0

0.524

0.2

FinalVolume

(mL)

100

100

100

50

100

100

50

100

Final Cone.(mg/L)

10,000

15,000

10,000

15,000

10,000

15,000

10,000

2000

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-0002METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. Q.608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page 18 of 35

SURROGATE WORKING STANDARD PREPARATION


SOP No. NC-OP-OQQ2Revision No. 0_Revision Date: 10/11/95Page 19 of 35

Table 2 Surrogate Working Standard Preparation

Type

BNA

Pest/PCBWorkingStockStandard

Pest/PCB

Compound

2-Flurobiphenyl

2-Fluorophenol

Nitrobenzene-d5

Phenol-d6

p-Terphenyl-dI4

2,4,6-Tribromophenol

Dibutylchlorendate


Dibutylchlorendate


Solvent

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Acetone

Acetone

Acetone

Acetone

SourceCone.(mg/L)

10,000

20,000

10,000

20,000

10,000

20,000

5000

2000

2000

200

AmountAdded(mL)

1.0

1.0

1.0

1.0

1.0

1.0

8

2

0.1

0.1

FinalVolume

(mL)

100

100

100

100

100

100

20

20

200

200

FinalCone.(mg/L)

100

150

100

150

100

150

2000

200

1

0.1

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OQQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page20_fiH5_

STOCK SPIKING STOCK SOLUTION PREPARATION


SOP No. NC-OP-OQQ2Revision No. Q_Revision Date: 10/11/95Page2J_oH5_

Table 3 Stock Spiking Stock Solution Preparation

Type

TCL BNA

BNA APPIX

BNA APPIX

Compound

Acenaphthene

4-Chloro-3 -Methylphenol

2-Chlorophenol

1 ,4-Dichlorobenzene

2,4-Dinitrotoluene

4-Nitrophenol

N-Nitroso-Di-n-Propylamine

Pentachlorophenol

Phenol

Pyrene

1 ,2,4-Trichlorobenzene

2-Acetylaminofluorine

4-Aminobiphenyl

Diallate

p-(Dimethylamino)azobenzene

Dinoseb

Disulfoton

3 -Methylcholanthrene

Solvent

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Neat Mass

g

1.0

2.0

2.0

1.0

1.0

2.0

1.0

2.0

2.0

1.0

1.0

0.10

0.10

0.10

0.10

1.0

0.10

0.10

FinalVolume

mL

100

100

100

100

100

100

100

100

100

100

100

10

10

10

10

10

10

10

FinalCone.mg/L

10,000

20,000

20,000

10,000

10,000

20,000

10,000

20,000

20,000

10,000

10,000

10,000

10,000

10,000

10,000

20,000

10,000

10,000


SOP No. NC-OP-0002Revision No. 0_Revision Date: 10/11/95Page22_oH5_

Type

BNANPDES

Compound

Phenacetin

Tetraethyldithiopyrophosphate

HC BASE/NEUTRALS MIX 1

Bis(2-chloroethoxy)methane

Bis(2-chloroethyl)ether

Bis(2-ethylhexyl)phthalate

Bis(2-chloroisopropyl)ether

4-Bromophenylphenylether

Butyl benzyl phthalate

4-Chlorophenylphenyl ether

Diethyl pohthalate

Dimethyl phthalate

Di-n-butyl phthalate

Di-n-octyl phthalate

N-Nitrosodimethylamine* *


N-Nitrosodiphenylamine* *

HC-BASE/NEUTRALS MIX 2

Azobenzene**

2-Chloronaphthalene

Solvent

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Neat Massg

0.10

0.10

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

FinalVolume

mL

10

10

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

FinalCone.mg/L

10,000

10,000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000


SOP No. NC-OP-Q002Revision No. flRevision Date: 10/11/95Page 24 of 35

Type Compound

Benzo(k)fluoranthene

Chrysene

Dibenzo(a,h)anthracene

Fluoranthene

Fluorene

Indeno (l,2,3-cd)pyrene

Naphthalene

Phenanthrene

Pyrene

HC PHENOLS MIX

4-Chloro-3-Methylphenol

2-Chlorophenol

2,4-Dichlorophenol

2,4-Dimethylphenol

2-Methyl-4, 6-Dinitrophenol

2-Nitrophenol

4-Nitrophenol

Pentachlorophenol

Phenol

2,4,6-Trichlorophenol

Solvent

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Neat Massg

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

FinalVolume

mL

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

FinalCone.mg/L

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000


SOP No. NC-OP-OQ02Revision No. Q_Revision Date: 10/11/95Page2icH5_

Type

Pest

Compound

HC BENZIDINE MIX

Benzidine**

3 ,3-Dichlorobenzidine

HC HAZARDOUSSUBSTANCE MIX 1

Benzoic acid

2-Methylphenol

4-Methylphenol



Aniline

Benzyl alcohol

4-Chloroaniline

Dibenzofuran

2-Methylnaphthalene

2-Nitroaniline

3-Nitroaniline

4-Nitroaniline

Aldrin

gamma-BHC-(Lindane

Solvent

Methanol

Methanol

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Acetone

Acetone

Neat Massg

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

0.10

0.10

FinalVolume

mL

1

1

1

1

1

1

1

1

1

1

1

1

1

1

50

50

FinalCone.mg/L

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000


SOP No. NC-OP-0002Revision No. Q_Revision Date: 10/11/95Page 25 of 35

Type

Pest

Compound

HC BENZIDINE MIX

Benzidine**

3,3-Dichlorobenzidine


Benzoic acid

2-Methylphenol

4-Methylphenol



Aniline

Benzyl alcohol

4-Chloroaniline

Dibenzofuran

2-Methylnaphthalene

2-Nitroaniline

3-Nitroaniline

4-Nitroaniline

Aldrin

gamma-BHC-(Lindane

Solvent

Methanol

Methanol

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

MeCl2

Acetone

Acetone

Neat Massg

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

0.10

0.10

FinalVolume

mL

1

1

1

1

1

1

1

1

1

1

1

1

1

1

50

50

FinalCone.mg/L

: ' . - . .

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000


SOP No. NC-OP-QOQ2Revision No. QRevision Date: 10/11/95Page26_oH5_

Type

PestNPDES

PCB

Compound

4,4'-DDt

Dieldrin

Endrin

Heptachlor

Methoxychlor

Aldrin

alpha-BHC

beta-BHC

delta-BHC

gamma-BHC-(Lindane

4,4' - DDD

4,4' - DDE

4,4' - DDT

Dieldrin

alpha-Endosulfan

Endosulfan Sulfate

Endrin

Heptachlor

Heptachlor Epoxide

PCB 1248

Solvent

Acetone

Acetone

Acetone

Acetone

Acetone

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Methanol

Dioxane

Dioxane

Methanol

Methanol

Methanol

Acetone

Neat Mass

g

0.10

0.50

0.25

0.10

0.20

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

N/A*

0.2

FinalVolume .

mL

0.25

100

50

50

50

1

1

1

1

1

1

1

1

1

1

1

1

1

1

100

FinalCone.mg/L

5000

5000

5000

2000

2000

5000

2500

2500

1000

1000

5000

5000

5000

1000

1000

1000

5000

5000

2500

2000


SOP No. NC-OP-OQ02Revision No. QRevision Date: 10/11/95Page 27 of 3 5

Type

TPH by GC

Compound

N-Dodecane

N-Hexadecane

N-Nonane

Solvent

Acetone

Acetone

Acetone

Neat Massg

1.0

1.0

1.0

FinalVolume

mL

100

100

100

FinalCone.mg/L

10,000

10,000

10,000

*Commercially prepares stock solution. Single and multiple compound solutions are purchased and notprepared in-house, hence neat mass is not applicable.

** These compounds are not required for the NPDES spike, but are normally included hi thecommercially prepared mixtures.

NOTE: All solutions containing more than one compound are labeled.

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTION SOP No. NC-OP-OOQ2METHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS Revision No. 0_608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 Revision Date: 10/11/95

Page28_cO5.

MATRIX SPIKE WORKING SOLUTION PREPARATION


SOP No. NC-OP-QOQ2Revision No. 0_Revision Date: 10/11/95Page 29 of 3 5

Table 4 Matrix Spike Working Solution Preparation

Type

TCL BNA

BNA APPIX

Compound

Acenaphthene

4-Chloro-3-Methylphenol

2-Chlorophenol


2,4-Dinitrotoluene

4-Nitrophenol


Pentachlorophenol

Phenol

Pyrene


2-Acetylaminofluorine

4-Aminobiphenyl

Diallate

p-(Dimethylamino)azobenzene

Dinoseb

Disulfoton

3-Methylcholanthreme

Solvent

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

SourceCone.mg/L

10,000

20,000

20,000

10,000

10,000

20,000

10,000

20,000

20,000

10,000

10,000

10,000

10,000

10,000

10,000

20,000

10,000

10,000

AmtAdded

mL

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

FinalVolume

mg/L

100

100

100

100

100

100

100

100

100

100

100

50

50

50

50

50

50

50

FinalCone.mg/L

100

200

200

100

100

200

.100

200

200

; 100100

1 00

100.

; IOC"

100

200

]00

100


SOP No. NC-OP-OQQ2Revision No. QRevision Date: 10/11/95Page 30 of 35

Type

BNANPDES

Compound

Phenacetin

Tetraethyldithiopyrophosphate


Bis(2-chloroethoxy)methane

Bis(2-chloroethyl)ether

Bis(2-ethylhexyl)phthalate

Bis(2-chloroisopropyl)ether

4-Bromophenylphenyl ether

Butyl benzyl phthalate

4-Chlorophenylphenyl ether

Diethyl phthalate

Dimethyl phthalate

Di-n-butyl phthalate

N-Nitrosodimethylamine


N-Nitrosodiphenylamine


Azobenzene

2-Chloronaphthalene


Solvent

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

SourceCone.mg/L

10,000

10,000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

AmtAdded

mL

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

FinalVolume

. mg/L

50

50

20 :

20

20

20

20

20

20 : "

; 20 ^

20

20

20

20

20

20

20

20 -

FinalCone.mg/L

100

• 100

100

100

100

100

100

: 100

100

100

100

100

100

100

100

100

100

100


SOP No. NC-OP-0002Revision No. QRevision Date: 10/11/95Page 3_LoH5_

Type Compound



2,4-Dinitrotoluene

2,6-Dinitrotoluene

Hexachlorobenzene

Hexachlorobutadiene

Hexachlorocyclopentadiene

Hexachloroethane

Isophorone

Nitrobenzene


HC POLYNUCLEARAROMATICHYDROCARBONS MIX

Acenaphthene

Acenaphthylene

Anthracene

Benzo(a)anthracene

Benzo(b)fluoranthene

Benzo(g,h,i)perylene

Benzo(k)fluoranthene

Solvent

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

SourceCone.mg/L

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

AmtAdded

mL

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

FinalVolume

mg/L

20

20

20

20

20

20

20

20

20

20

20

20

20

20

20

20

20

20

FinalCone.mg/L

100

100

100

- 100

100

100

100

100

100

100

100

100

100

100

100

"100

100

100


SOP No. NC-OP-QQQ2 '-Revision No. P_Revision Date: 10/1-1795'Page3_2_2H5_

Type Compound

Chrysene

Dibanzo(a,h)anthracene

Fluoranthene

Fluorene

Indeno( 1 ,2,3-cd)pyrene

Napthalene

Phenanthrene

Pyrene

HC PHENOLS MIX

4-Chloro-3-Methylplhenol

2-Chlorophenol

2,4-Dichlorophenol

2,4-Dimethylphenol

2,4-Dinitrophenol

2-Methyl-4,6-Dinitrophenol

2-Nitrophenol

4-Nitrophenol

Pentachlorophenol

Phenol


Solvent

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

SourceCone.mg/L

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

AmtAdded

mL

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0 .

FinalVolume

mg/L

20

20

20

20

20

20

20

20

20 .

i 20

20

20

20

20

20

20

20

20

20

FinalCone.mg/L

100

100

100

100

100

100

100

,100

*100

,100

- 100

100

100

100

100

100

100

100

100


SOP No. NC-OP-0002Revision No. QRevision Date: 10/11/95

Type

Pest

Compound

HC BENZIDINE MIX

Benzidihe

3 ,3 -Dichlorobenzidine

HC HAZARDOUSSUBSTANCE MDC 1

Benzoic acid

2-Methylphenol

4-Methylphenol


HC HAZARDOUSSUBSTANCE MDC 2

Aniline

Benzyl alcohol

4-Chloroaniline

Dibenzofuran

2-Methylnapthalene

2-Nitroaniline

3-Nitroaniline

4-Nitroaniline

Aldrin

gamma-BHC (Lindane)

Solvent

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

MeOH

Acetone

Acetone

SourceCone.mg/L

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

2000

AmtAdded

mL

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

1.0

LO

1.0

1.0

1.0

0.01

0.01

FinalVolume

mg/L

20

20

20

20

20

20-

20

20

20

20

20

20

20

20

100

100

FinalCone.mg/L

100

100

100

100

100

100

100

100

100

100

100

100

100

100

0,2

0.2

SEPARATORY FUNNEL LIQUID/LIQUID EXTRACTIONMETHOD 3510 FOR BNA/PAH 625/8270 PESTICIDE/PCBS608/8080 TPH BY GC OPP 8141 PAHS 8100, 8310 -

SOP No. NC-OP-OQ02 IRevision No. Q.Revision Date:-10/11/95Page 34 of 35

, Type

Pest DrinkingWater

PestNPDES

Compound

4,4'-DDT

Dieldrin

Endrin

Heptachlor

gamma-BHC (Lindane)

Endrin

Methoxychlor

Aldrin

alpha-BHC

beta-BHC

delta-BHC

gamma-BHC (Lindane)

4,4'-DDD

4,4'DDE

4,4'-DDT

Dieldrin

alpha-Endosulfan

beta-Endosulfan

Endosulfan Sulfate

Solvent

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

SourceCone.mg/L

5000

500

5000

2000

2000

5000

2000

5000

2500

2500

1000

1000

5000

5000

5000

1000

1000

1000

1000

AmtAdded

mL

0.01

0.10

0.01

0.01

0.005

0.005

0.025

0.04

0.08

0.08

0.20

0.20

0.20

0.04

0.20

0.20

0.20

1.0

1.0

FinalVolumemg/L

100

100

100

2000

50

50

50

100

100

100

100

100

100 /

100

100

100

100

100

100

,, FinalCone.mg/L

0.5

0.5

., 0.5

0.2

0'.2

0.5.

1.0

" ••'.'' J2: '

/ '2

: .. 2 '

^:,2'-2

,.10

2

10

2

2

10

10


SOP No. NC-OP-OOQ2Revision No. QRevision Date: 10/11/95Page 35 of 35

Type

PCB

TPHbyGC

Compound

Endrin

Heptachlor

Heptachlor Epoxide

PCB 1248

N-Dodecane

N-Hexadecane

N-Nonane

Solvent

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

Acetone

SourceCone.mg/L

5000

5000

5000

0.2

1.0

1.0

1.0

AmtAdded

mL

0.20

0.04

0.08

100

100

100

100

FinalVolume

mg/L

100

100

100

2000

10,000

10,000

10,000

FinalCone.mg/L

10

10

10

20

1000

1000

1000

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