# Attachment D

Sampling and Analysis Plan

# Sampling and Analysis Plan F037 Waste Delisting

Prepared for:

ConocoPhillips Company Billings Refinery 401 South 23rd Street Billings, Montana 59101

Prepared by:

TRC Environmental Corporation 505 East Huntland Drive, Suite 250 Austin, Texas 78752

TRC Project No. 172405

June 2010Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 Table of Contents 

## Table of Contents Page

1.0 Objectives of the Sampling Effort ....................................................................... 1-1

2.0 Description of the Waste to be Sampled..............................................................2-1

3.0 Description of the Sampling Strategy..................................................................3-1

4.0 Sampling and Analytical Requirements...............................................................4-1Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 1-1 

### 1.0 OBJECTIVES OF THE SAMPLING EFFORT

This document presents the proposed Sampling and Analysis Plan (SAP) to support F037 waste delisting for residual solids generated from the oil-recovery process for secondary oil-bearing hazardous materials at the ConocoPhillips (COP) Billings, Montana Refinery (“the Refinery”).

The ConocoPhillips Refinery is located at 401 South 23rd Street in Billings, Montana and covers approximately 200 acres on the southeastern side of Billings. The legal description of the Refinery is Northwest 1⁄4 of Section 2, Township 1 South, Range 26 East in Yellowstone County, Montana. The Refinery, which began operations in 1949, currently converts crude oil and condensate, as well as field butane, by various processes into liquid petroleum gases, gasoline, jet fuel, diesel fuel, fuel oils, asphalt, and petroleum coke.

As part of current operations at the Refi nery, sludge is periodically removed from two storm water tanks and processed via centrif uge and/or filter press for oil recovery and dewatering. The residual solids from the oil-recovery process are characterized as F037, a hazardous waste under the Resource Conservation and Recovery Act (RCRA). COP is petitioning the United States Environmental Protection Agency (US EPA), Region 8, to exclude from hazardous regulation (i.e., delist), the tank residuals that are currently being managed as F037 wastes. This SAP has been prepared to guide the analytical program that will be conducted in support of the delisting determination.

The objective of the sampling effort is to obtain waste characterization data that
demonstrates:

• The residual solids do not meet the criteria for which F037 wastes are listed;

• The residual solids do not exhibit a characteristic of a hazardous waste; and

• The waste does not contain any other constituents at levels of concern.

The proposed delisting would authorize periodic disposal of the wastes at a permitted RCRA Subtitle D solid waste landfill. ConocoPhillips is requesting delisting for approximately 500 tons (measured on a wet weight basis) of residuals per year. Although the cleaning cycle for these tanks averages about once every 18-24 months, and the volume of residuals is generally less than 500 tons, use of the higher value and annual frequency will allow for management of all residuals under the delisting and ensure that disposal is protective of human health and the environment.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 2-1 

### 2.0 DESCRIPTION OF THE WASTE TO BE SAMPLED

Residual solids are generated when sludge is removed from two tanks that receive storm water runoff from the Refinery proce ss area, as well as some dry-weather flow consisting of water from washdown and maintenance and cleaning activities, steam condensate, and heat exchanger back-flushing. The sludge from the tanks meets the definition for listing as a hazardous waste, specifically as primary sludge (F037), perTitle 40 of the Code of Federal Regulations (40 CFR), Section (§) 261.32. The colocated, in-ground concrete tanks are approxima tely 30-feet (ft) wide by 130-ft long by 8- ft deep, with each having a capacity of approximately 175,000 gallons. The tanks are separated by a concrete wall running east-west . Figure 2-1 depicts the configuration of the tanks. Figure 2-2 depicts the dimensions of the tank. The tanks are a part of the Refinery’s Clean Water Act (CWA)-permitted wastewater system. Liquids in the tanks are normally directed to the facility wastewater treatment plant and are not part of the proposed delisting. Sludge from the tanks is periodically removed, de-oiled and dewatered using a refinery filter press (and/or with an additional portable centrifuge), and the residual solids are shipped off-site as F037 waste. Initial sampling data does not indicate any hazardous characteristic levels for toxicity characteristic (TC) constituents (40 CFR §261.24). Recovered oil is reinserted into the refining process and water from dewatering is routed to the Refinery’s on-s ite wastewater treatment plant for discharge via the Refinery’s CWA discharge permit.

Tank flow is presented in Figure 2-3. Flow from the refinery’s process area storm sewer system enters the south tank at its northwestern corner via an underground pipe. Incidental run-off from the filter press area enters the north tank at its northwestern
corner. Flow from the south tank enters the north tank via a valve located at the bottom of the dividing wall between the tanks along the eastern side of the wall. Floating suction
at the northeastern corner of the north tank directs water to the wastewater treatment
system.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 2-2 

### Figure 2-1. The Tanks

Figure 2-2. Tank Dimensions 30-ft

30-ft 130-ft 8-ftSampling and Analysis PlanF037 Waste DelistingConocoPhillips Company, Billings RefineryJune 2010Project No. 1724052-3Figure 2-3. Tank FlowProcess AreaStorm SewerSystem(Underground)Run-Off fromFilter PressAreaProcess Area Storm Water Tank-NorthNormally open connecting valve located atbottom of dividing wallNormal Routing:To WastewaterTreatment SystemNorthProcess Area Storm Water Tank - SouthFloatingSuctionSampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 3-1 

### 3.0 DESCRIPTION OF THE SAMPLING PROGRAM

The sampling program will consist of one sampling event. Eight (8) samples, one (1) duplicate, and one matrix spike/matrix spike duplicate (MS/MSD) pair will be collected of the filter-pressed material for both totals and Toxicity Characteristic Leaching Procedure (TCLP) analyses of the constituents of concern (COC) list provided
in Section 4.0. The COC list consists of a subs et of the Appendix IX constituent list in 40 CFR Part 264, and is based on: 1) knowledge of Refinery processes and wastes; 2) the evaluation of available references, including Exhibit 3 of the March 23, 2000 USEPA RCRA Delisting Program Guidance Manual for the Petitioner entitled Constituents of Concern for Wastes from Petroleum Processes ; 3) the USEPA Region 5 “Skinner List” constituents (i.e., those constituents commonly found in Refinery wastes and updated to address toxicological and analytical concerns); and 4) the basis for listing constituents for F037 per 40 CFR Part 261 Appendix VII (i.e., benzene, benzo(a)pyrene, chrysene, lead, and chromium). Each sample will also be an alyzed for pH, oil & grease, total cyanide, and sulfide levels. Samples will not be analyzed for ignitability or corrosivity since these characteristics are not applicable to solids. Two samples of the filter-pressed material (one from pressed sludge from each tank) will be analyzed using the additional neutral and alkaline pH TCLP extraction fluids presented in the delisting guidance.

Characterization of Spatial and Temporal Variability Sampling will adequately characterize both spatial and temporal variability. The samples will be collected in the spring/summer of 2010, approximately eight months following the most recent tank cleanout. This time frame will allow for sufficient accumulation of refinery wastewater/sludge materials in the tanks to account for temporal variability. Specifically, the material is deposited in the tanks primarily during storm events and maintenance/cleaning activities. Thus, the deposition of specific COCs will be random with respect to the generating event. By allowing an eight-month accumulation window, representative collection of material normally entering the tanks will be
achieved.

To account for spatial variability, each tank will be divided into four quarters along the 130-ft dimension and sludge will be drawn from a full vertical profile (i.e., from the top of the sludge to the bottom of the tank) at four locations within each quarter. The distribution of the COCs within the tank quarters is expected to be random based on the events contributing to the deposition of material.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Company, Billings Refinery June 2010

Project No. 172405 3-2 

### Sludge Collection Strategy The sludge collection strategy is designed to mimic actual tank clean-out procedures. These include:

1. A vacuum truck will be utilized for sludge recovery from the tanks

2. The hose/nozzle assembly of the vacuum truck will be lowered through the water column to collect material from the top of the sludge to the bottom of the tank (i.e., a full vertical profile)

3. Sludge will be collected from at least four locations within each tank quarter

4. Solids will be removed from the vacuum truck and placed in the mix tank of the filter press

5. Approximately 50 barrels of material will be processed through the filter press

6. Samples of the filter pressed material will be collected for laboratory
submission

7. The filter press and vacuum truck will be cleaned between sludge collection/processing from each tank quarter

Sludge Collection Team Paul Lemire will provide sludge collection and sampling oversight for this project. Technicians will be Michael Ewer t and Michael Connoly. Current resumes for these individuals are presented in Attachment A to this document.

Sludge Collection Locations Each tank will be divided into quarters along the 130-ft wall. Each quarter will measure approximately 32.5-ft by 30-ft. Each quarter will be divided into thirds along each side (i.e., 10-ft intervals along the 30- ft dimension and 10.8-ft intervals along the 32.5-ft dimension) with sludge collected at the intersections of these lines. Approximate sludge collection locations are shown in Figure 3-1.

Sludge collection locations within each tank may be re-located based on availability of material; however, collection locations will remain within each tank quarter and, at a minimum, sludge will be collected from four locations within each
quarter.

Health and Safety Procedures All sludge collection activities will be conducted in accordance with the Refinery’s approved RCRA Corrective Action Site wide Health and Safety Plan (HASP).Sampling and Analysis PlanF037 Waste DelistingConocoPhillips Company, Billings RefineryJune 2010Project No. 1724053-3= Approximate Sample Collection LocationFigure 3-1. Sample Collection LocationsProcess Area Storm Water Tank - NorthNorthProcessAreaStorm Water Tank -South32.5-ft32.5-ft32.5-ft32.5-ftSouthQ1SouthQ2SouthQ3SouthQ4NorthQ1NorthQ2NorthQ3NorthQ4Sampling and Analysis PlanF037 Waste DelistingConocoPhillips Company, Billings RefineryJune 2010Project No. 1724053-4Table 3-1. Anticipated SamplesTotalTCLP4SamplesVOCs1SVOCs1Metals1Cyanide2Sulfide3Oil &GreasepHMoistureAcid5Neutral6Basic7NorthQ1999999999-- --NorthQ2999999999-- --NorthQ3999999999-- --NorthQ49999999999898SouthQ19999999999898SouthQ2999999999-- --SouthQ3999999999-- --SouthQ4999999999-- --Field Duplicate9999999999-- --MS10999999--99-- --MSD10999999--99-- --1 See Table 4-1 for target analyte listsfor volatile organic compounds (VOCs), semivolatile organic compounds (SVOCs) and metals including mercury.2 Total and amenable cyanide – Methods 9014/9213.3 Methods 9034/92154 TCLP analyses will be required for VOCs, SVOCs, and metals including mercury.5 “Acid” refers to the extraction fluid pH as determined using Method 1311.6 “Neutral” refers to the extraction fluid pH (DI water).7 “Basic” refers to the extraction fluid pH (according toStandard Methods for the Examination of Water and Wastewater).8 Sample material (filter-pressed material)from two quarters (one from each tank) willbe submitted for TCLP analyses using the additional neutral and basicextraction fluids. Based on previous experience, sample material from filter-pressed sludge from NorthQ4and SouthQ1 are selected for the extra TCLPextractions and analyses. The specific locations of these samples may be altered based on the availability of sludge and/or any other mitigating factor.9 Extra filter-pressed sample material from onelocation will be submitted as a field duplicate.10 Extra filter-pressed sample material from one location will be submitted for matrixspike (MS) analyses and duplicate MS (MSD) analyses.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 1 

### 4.0 SAMPLING AND ANALYTICAL REQUIREMENTS

The overall quality objective is to implement procedures that will provide scientifically valid results that are sufficient to meet the objectives of the sampling

program.
Table 4-1 presents analytical method and targeted reporting limits for metals, total and amenable cyanide, and organic analytes.

Order of Sample Collection Samples for volatile organics must be collected immediately following filter press processing and compositing of the grab samples in order to minimize the loss of target analytes. The remaining samples will be collected in the following order: semivolatile organics, oil & grease, metals, cyanide, and the remaining parameters.

Sample Collection Protocol Four independent grab samples will be co llected from each batch (each quarter) of filter-pressed material. These grab samples will be composited and placed into appropriate containers for submission to the laboratory (see Table 4-2).

Sample Numbering The following items will be used to name samples:

• Sample material will be collected from filter-pressed sludge

• The filter press will process sludge from each tank quarter

• There is a north tank and a south tank

Therefore, samples will be named according to the tank and quarter from which the material was collected (with quarters being numbered 1-4 from east to west [see Figure 3-1]). For example, the sample collected from the third quarter of the north tank will be named NorthQ3.

Field duplicates will be numbered by adding a 2 to the end of the sample name. For example, if a field duplicate is collected from the first quarter of the south tank, then the original sample would be named SouthQ1 and the field duplicate would be named SouthQ12.

Trip blanks will be named beginning with a “TB”, followed by the date collected, and including consecutive letters. For example, the first trip blank submitted on May 1,Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 2 

### 2010 would be named TB050110A, the second trip blank submitted on the same day would be named TB050110B, etc.

Sample Containers and Preservation Holding times, preservation requirements, and typical containers for solid samples, are presented in Table 4-2.

Sample Documentation Specific procedures for chain-of-custody will be in accordance with the Refinery’s Standard Operating Procedures (SOPs).

Sample Shipment A completed COC form will accompany samples during each step of custody transfer and shipment. When physical possession of samples is transferred, both the individual relinquishing the samples and the individual receiving them will sign, date, and record the time on the COC form. In the case of sample shipment by an overnight courier, a properly prepared air bill (waybill) will serve as an extension of the COC form while the samples are in transit.

The following steps must be followed when packing environmental samples for shipment by air:

1. Select a sturdy cooler in good condition. Secure and tape the drain plug with duct tape.

2. Ensure the caps on all bottles are tight (will not leak); check to see that labels and chain-of-custody records are completed properly.

3. Place all bottles in separate and appropriately sized plastic zip-top bags and close the bags. Bottles may be wrapped in bubble wrap. It is preferable to place glass sample bottles and jars into the cooler vertically. Due to the strength properties of a glass container, there is much less chance for breakage when the container is packed vertically rather then horizontally.

4. Place two to four inches of packing peanuts, vermiculite, or other cushioning material into the bag in the cooler and then place the bottles and cans in the bag with sufficient space to allow for the addition of more packing peanuts or
vermiculite between the bottles and cans.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 3 

### 5. Put ice in large plastic zip-top bags and properly seal. Place these ice bags on top of and between the samples. Fill all remaining space between the bottles or cans with packing peanuts, bubble wrap, or vermiculite.

6. Place the completed Chain-of-Custody Record into a plastic zip-top bag, tape the bag to the inner side of the cooler’s lid, and then close the cooler.

7. Wrap strapping tape around each end of the cooler two times, and completed custody seals affixed to the top on adjacent sides of the cooler. Place the custody seals so that the cooler cannot be opened without breaking the seal. Place clear shipping tape over the custody seals.

8. A label containing the name and address of the shipper shall be placed on the outside of the container, preferably using a handle-tag or secured with extra tape across the top of the cooler.

Laboratory ALS Laboratory Group in Houston, Texas will perform analyses associated with this project.

• The laboratory contact is Hector Coronado

• The telephone number is (281) 530-5656

Toxicity Characteristic Leaching Procedure (TCLP) Samples will be analyzed for both total and TCLP volatiles, semivolatiles, and metals. Regarding TCLP analyses, all samples will be extracted using the appropriate extraction fluid as determined using TCLP method (SW846 Method 1311) criteria and procedures. Additionally, sufficient filter-pressed sample material of sludge from one quarter of each tank (i.e., NorthQ4 and SouthQ1) will be extracted using extraction fluids with pH values of 7.0 and 10.1 (as noted in delisting guidance documents) with subsequent analyses for volatiles, semivolatiles, and metals. The laboratory must be contacted well in advance of receiving samples to discuss the generation and use of these
non-standard extraction fluids.

The extraction fluid with a neutral pH is described in Method 1311, Section 5.2 as reagent water and has a pH of 7.0 ± 0.5 standard units.

The extraction fluid with an alkaline pH is described in Standard Methods for the Examination of Water and Wastewater . It is prepared by mixing 2.092 grams of 0.025 molar sodium bicarbonate (NaHCO 3 

### ) and 2.640 grams of 0.025 molar sodium carbonateSampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 4 

### in 1000 mL aqueous solution at 25°C. This solution must have a pH of 10.01 ± 0.05
standard units.

Reporting Limits A majority of the critical delisting levels are expected to be determined primarily for the groundwater ingestion pathway. Ther efore, obtaining data with the lowest possible reporting limits is of utmost importance – especially for TCLP results. Since the sample matrix is sediment, target reporting limits are likely to be unattainable. Every effort must be made by the laboratory to report the lowest practical reporting limit.

Table 4-1 presents analytical method and targeted reporting limits for metals, total and amenable cyanide, and organic analytes.

Quality Control Samples As previously discussed, the residual solids are not expected to show significant variability and should be relatively homogeneous. Combined sampling and analytical variability will be measured by the collection of a duplicate sample. The field duplicate will be collected by filling two sets of sample containers from the composite sample of one batch of material processed through the filter press.

A trip blank will be used to assess sample container and potential transportation impacts.

A matrix spike/matrix spike duplicate pair (MS/MSD) will be collected and analyzed to assess analytical precision and accuracy.

All quality control (QC) samples will be collected in accordance with the frequencies in Table 4-3

Decontamination Prior to sample collection and processi ng, the filter press and vacuum truck will be decontaminated. Generally, refinery e ffluent water will be processed through the vacuum truck and filter press for decontamination purposes. The filter press and vacuum truck will also be decontaminated between collection at tank quarters.

If disposable equipment is used for sampling, each location will have dedicated equipment that will be used for one sample, then discarded. If non-disposable equipment is used, any other equipment that might come into contact with the sample will be thoroughly decontaminated prior to taking the first sample and between tank quarters. This decontamination procedure includes the following steps:Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 5 

### 1. Lay out sufficient polyethylene shee ting on the ground or floor to allow placement of the equipment being decontaminated.

2. Remove non-aqueous phase liquids (NAPL), if present, with an absorbent pad or
other suitable device.

3. Remove any solid material (to the degree possible) with a brush and potable tap or
distilled water.

4. Wash the equipment with a brush, la boratory grade non-phosphate detergent (e.g., Liquinox, Alconox), and potable tap or distilled water.

5. Rinse the equipment with potable tap or distilled water.

6. Rinse the equipment with 10 percent methanol.

7. Rinse the equipment with distilled water.

8. Reassemble equipment, if necessary, and wrap completely in clean, unused aluminum foil, shiny side out for transpor t and/or storage. Re-use of equipment on the same day without wrapping in foil is acceptable.

Record all decontamination procedures in the field logbook or appropriate field form.

A list of potential sample collection equipment is provided in Table 4-4.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 6 

### Table 4-1. Analytical Methods and Target Reporting Limits

Analyte Method Total Target Reporting Limit (mg/kg) 1 

### TCLP Target Reporting Limit (mg/L) 1 

### Inorganics Antimony 0.5 0.005 Arsenic 0.5 0.005 Barium 0.5 0.005 Beryllium 0.5 0.005 Cadmium 0.5 0.005 Chromium 0.5 0.005 Cobalt 0.5 0.005 Lead 0.5 0.005 Nickel 0.5 0.005 Selenium 0.5 0.005 Silver 0.5 0.005 Vanadium 0.5 0.005 Zinc 6010; 6020

0.5 0.005 Mercury 7471 0.005 0.0002 Volatile Organics Benzene 0.005 0.005 Carbon disulfide 0.010 0.010 Chlorobenzene 0.005 0.005 Chloroform 0.005 0.005 1,2-Dichlorobenzene 2 

### 0.005 0.005 1,3-Dichlorobenzene 2 

### 0.005 0.005 1,4-Dichlorobenzene 2 

### 0.005 0.005 1,2-Dichloroethane 0.005 0.005 1,1-Dichloroethane 0.005 0.005 1,1-Dichloroethylene 0.005 0.005 1,4-Dioxane 0.10 0.10 Ethylbenzene 0.005 0.005 Ethylene dibromide 0.005 0.005 Methyl ethyl ketone 0.010 0.010 Methyl t-butyl ether 0.005 0.005 Naphthalene 2 

### 0.005 0.005 Styrene 0.005 0.005 Tetrachloroethylene 0.005 0.005 Toluene 0.005 0.005 1,1,1-Trichloroethane 0.005 0.005 Trichloroethylene 0.005 0.005 Xylenes (total) 8260

0.005 0.015Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 7 

### Table 4-1. Analytical Methods and Target Reporting Limits (continued)

Analyte Method Total Target Reporting Limit (mg/kg) 1 

### TCLP Target Reporting Limit (mg/L) 1 

### Semivolatile Organics Acenapthene 0.167 0.005 Anthracene 0.167 0.005 Benzo(a)anthracene 0.167 0.005 Benzo(a)pyrene 0.167 0.005 Benzo(b)fluoranthrene 0.167 0.005 Benzo(k)fluoranthene 0.167 0.005 Bis(2-ethylhexyl)phthalate 0.167 0.005 Butyl benzyl phthalate 0.167 0.005 Chrysene 0.167 0.005 o, m, p-Cresol 0.167 0.005 Dibenz(a,h)anthracene 0.167 0.005 Diethyl phthalate 0.167 0.005 Dimethyl phthalate 0.167 0.005 Di-n-butyl phthalate 0.167 0.005 2,4-Dimethylphenol 0.167 0.005 2,4-Dinitrophenol 0.167 0.005 2,4-Dinitrotoluene 0.167 0.005 Di-n-octyl phthalate 0.167 0.005 Fluoranthene 0.167 0.005 Fluorene 0.167 0.005 Indeno(1,2,3-cd)pyrene 0.167 0.005 Nitrobenzene 0.167 0.005 4-Nitrophenol 0.167 0.005 Phenanthrene 0.167 0.005 Phenol 0.167 0.005 Pyrene 0.167 0.005 Pyridine 0.167 0.005 Quinoline 8270

0.167 0.005

1 Reporting limits presented here represent ideal conditions. Actual limits will differ based on samplespecific factors (e.g., percent mo isture, dilution factor, etc.).

2 Analysis can be performed using Method 8260 or Method 8270.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 8 

### Table 4-2. Sample Handling Requirements

Analyte Method Typical Containers 1 

### Preservative Holding Time No. Samples 2


### Total and Amenable Cyanide 9014; 9213 4 ounce Glass Cool to 4°C 14 days 9 Hexane-Extractable Material (Oil & Grease) 9071 4 ounce Glass Cool to 4°C 14 days 9

Metals 6010; 6020 4 ounce Glass Cool to 4°C 180 days 9

Mercury 7471 4 ounce Glass 

### Cool to 4°C 28 days 9

Moisture Content ASTM D2216 4 ounce Glass 

### Cool to 4°C 28 days 9

pH 9045 4 ounce Glass Cool to 4°C 7 days 9

Semivolatile Organics 8270 4 ounce Glass Cool to 4°C 14 days to extraction;

40 days

from extraction to analysis 9

Volatile Organics 8260 4 or 8 ounce Glass Cool to 4°C 14 days 9

Sulfide 9034; 9215 4 ounce Glass Cool to 4°C; Zn Acetate until surface

moistened 

### 7 days 9

Reactive Sulfide SW-846 Chapter 7 4 ounce Glass Cool to 4°C 14 days 9

Reactive Cyanide SW-846 Chapter 7 4 ounce Glass Cool to 4°C 14 days 9

TCLP 1311 a 

### See Determinative Method pH 7.0 – 2 pH 4.93 – 9 pH-10.1 - 2

1 Containers presented here assu me one sample for one method is being submitted for analysis. The

laboratory may use larger containers and/or use th e material from one contai ner for multiple methods. Contact the laboratory for specific advice regarding containers.

2 The number of samples listed here include eight (8) samples plus one (1) field duplicate. Sufficient

sample material from one (1) location will also be submitted to the laboratory for MS/MSD analyses for all analytes excluding TCLP using extraction fluids at pH values of 7.0 and 10.1.

a Per delisting guidance, TCLP must be performed us ing a minimum of three different extraction fluids

in a pH range from 3-11 (i.e., 4.93, 7.0, and 10.01). Two (2) samples will require extraction using these three fluids (i.e., the remaining six (6) samples will be extracted using the one fluid described in Method 1311). Contact the laboratory prior to sample collection to discuss this modification to the TCLP method.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 9 

### Table 4-3. QC Sampling Frequencies

QC Sample Type Frequency Field Duplicate 5 % a 

### Matrix Spike/Matrix Spike Duplicate Pair 5 % a



### Trip Blanks 1 

### One per cooler containing samples for volatile organic analyses a 5 % frequency means one QC sample (or one MS/MSD pair) is collected for every twenty or fewer field samples.

1 Trip blanks are only analyzed for volatile organic target compounds.Sampling and Analysis Plan F037 Waste Delisting ConocoPhillips Billings, Montana, Refinery June 2010

Project No. 172405 4- 10 

### Table 4-4. Potential Sample Collection Equipment

Item Purpose Sample Collection Equipment FRP Coveralls Safety Steel-Toed Boots Safety Hard Hats Safety Safety Glasses Safety Hearing Protection Safety Nitrile Gloves Outer Gloves Blue Mesh Sample Protection Visqueen ® Plastic Sheeting Sample Protection Stainless Steel Bowls Sample Containment Stainless Steel Scoops Sample Manipulation Coolers Sample Storage and Shipment Ice Sample Preservation Laboratory Supplied Containers Sample Containers Decontamination Equipment Laboratory Suitable Detergent Decontamination Distilled Water Soapy Water and Pre-Wash Water 10% methanol Solvent Rinse Distilled Water Final Rinse Buckets Contain Pre-Wash and Soapy Water Brushes Scrubbing Visqueen ® Plastic Sheeting Contain Accidental Spills Shipping Supplies Chain-of-Custody Forms Documenting Individual Sample Information Sample Labels Container Contents Identification Absorbent Paper Sample Packing Shipping Labels Laboratory Address Sample Analysis and Target Analyte Lists Laboratory Notification Overnight Carrier Shipping Forms Timely Delivery Custody Seals Indicator of Tampering With Cooler “Fragile” Labels Proper Handling of Cooler “This Side Up” Labels Proper Handling of Cooler Packing Peanuts or Vermiculite Sample Packing Clear Tape Shipping Label Protection Reinforced Tape Ensuring Cooler Closure Resealable Plastic Bags Ice and Documentation Containment

# Attachment A
Sampling Team ResumesTetra Tech Page 1 

## PAUL E. LEMIRE Senior Hydrogeologist / Project Scientist

EDUCATION MS, Hydrology, University of New Hampshire, 1982 BS, Zoology, Montana State University, 1976

REGISTRATIONS/CERTIFICATIONS Monitoring Well Constructor: Montana (#404, 2008)

EXPERIENCE SUMMARY Mr. Lemire has over 27 years of experience working on water resource and environmental projects for the insurance, oil and gas, wood preserving, and railr oad industries and governmental agencies. He has conducted soil and groundwater investigations for env ironmental emergency response action as well as Resource Conservation and Recovery Act (RCRA) hazardous waste sites; Comprehensive Emergency Response, Compensation and Liability Act (CERCLA) Superfund sites; and underground storage tank (UST) sites. Tasks have included environmental emergency res ponse on-site coordination, work plan preparation, monitoring well installation, soil sampling, groundwater monitoring, aquifer testing, groundwater modeling, and hydrogeologic and chemical data interpretation. Mr . Lemire has also served as an expert witness and negotiated with environmental regulator s on technical and compliance issues.

PROJECT EXPERIENCE Environmental Emergency Response

• Vehicle Diesel Spill, Yellowstone National Park. Project Manager/ER Coordinator responsible for directing several investigations and cleanup of diesel fuel spill from vehicle accidents in Yellowstone National Park. Excavated fuel-impacted soil and pr evented fuel from impacting nearby surface water bodies. All emergency response projects were closed by the Wyoming Dept. of Environmental Quality. (2002, 2003, 2006, 2008)

• Petroleum Pipeline Crude Oil Spill Emergency Response, Montana. As Senior Hydrogeologist, provided emergency response coordination of environment al efforts, conducted in vestigation of surface and subsurface petroleum impacts and proposed remediation measures. (2001)

• Petroleum Pipeline Diesel Fuel Spill Emergency Response, Montana. As Senior Hydrogeologist, provided response coordination, surface soil inve stigation efforts and prov ided proposed remediation measures. (2004)

• Tractor/Trailer Gasoline Spill Emergency Response, South-central Montana. Project Manager/ Senior Hydrogeologist responsible for directing a subsurface soil and groundwater investigation for a 4,000-gallon gasoline spill on a secondary highway. Ex cavated petroleum hydrocarbon-impacted soil, negotiated with local landowners for land treatment site, land-treated the soil to environmental agency cleanup levels and conducted a groundwater investigation. (2003)

• Tractor/Trailer Gasoline Spill Emergency Response, Southwestern Wyoming. Project Manager/ Senior Hydrogeologist responsible for directing a subsurface soil and groundwater investigation for a 12,000-gallon gasoline spill on a secondary highway. Ex cavated petroleum hydrocarbon-impacted soil, land-treated the soil at an off-site location to environmental agency cleanup levels and conducted a groundwater investigation. (2003)

• Tractor/Trailer Diesel Spill Emergency Response, Southwestern Wyoming . Project Manager/ Senior Hydrogeologist responsible for directing a subsurfa ce soil and surface water investigation for a 4,000- gallon diesel spill on a secondary highway. Excavated di esel-impacted soil, land-treated the soil at an offsite location to environmental agency cleanup levels and conducted a surface water investigation for diesel spills into a creek. (2003)Paul E. Lemire

Tetra Tech Page 2 • Carbon Tetrachloride Spill Emergency Response, Oklahoma . As Senior Hydrogeologist, directed a subsurface investigation of carbon tetrachloride in unconsolidated sediments and fractured bedrock. Spill resulted from a railroad derailment. (1996)

Remedial Investigation / Feasibility Study

• RCRA Facility Investigations (RFI) and Corrective Measures Studies at Oil Refineries, Montana. Project Manager/ Senior Hydrogeologist responsible fo r RFI and corrective measures studies at three Yellowstone County oil refineries. Work included insta llation of monitor wells, oil and dissolved chemical recovery wells, soil and groundwater investigations for solid waste management units, and land treatment unit investigations. Responsible for liaison and negotia tion with state and federal environmental agencies. (1991 to present)

• Oil Refinery RFI, Northwestern Washington . Project Manager/ Senior Hydrogeologist responsible for preparing the RFI work plan and implementing fieldwork to complete the first RFI in the United States. Work included installation of monitor wells, soil and groundwater investigations for solid waste management units, and land treatment unit investigati ons. Responsible for liaisons and negotiations with state and federal environmental agencies. (1993)

• Site Investigations/Remediation, Wood Preserving Facilities, Paradise and Somers, Montana. Principal Hydrogeologist responsible for site in vestigations and remediation at railroad tie wood preserving facilities. Installed over 40 monito r wells, conducted RCRA solid waste management unit investigations, conducted aquifer tests, designed and implemented creosote re covery systems using wells, and prepared RCRA Part B permits for a land treatment unit and waste management pile. Responsible for liaison and negotiation with st ate and federal environmental agencies. (1992)

• Site Investigation, Wood Preserving Facility, Kalispell, Montana . Principal Hydrogeologist responsible for site investigation at a post and pole wood preserving facility using pentachlorophenol. Installed monitor wells and conducted soil and gr oundwater investigations and agency negotiations. (1995)

• Petroleum Refinery Site Investigation, Louisiana. Senior Hydrogeologist responsible for the site investigation of an ethylene dichloride spill at petroleum refinery loading docks. (1995)

• Hazardous Waste Reviews, Wood Preserving F acilities, Florida, Georgia and Mississippi . As Principal Hydrogeologist, reviewed waste management at facility, disposal facilities, waste disposal volumes, RCRA hazardous waste review, and hydrogeol ogic setting of waste disposal facilities to determine RFI issues and quantity of solid waste management units and areas of concern. (1990)

• RI/FS and Site Clean-up, Used Oil Recyc ling Site, Yellowstone County, Montana . Project Manager/Senior Hydrogeologist responsible for RI/FS work plan preparation, the remedial investigation, and site cleanup for a Montana Superfund site. Subsur face soils and groundwater at the site were impacted with petroleum hydr ocarbons and heavy metals. (1996)

• RI/FS and Remediation, Metal Recycling Facility, Nebraska . Project Manager responsible for RI/FS investigation and remediation of subsurface soils and groundwater impacted by lead and sulfuric acid. (1992)

Environmental Site Assessments

• Phase I Environmental Site Assessments (ESAs), Montana and Wyoming . Project Manager/ Principle Investigative Officer responsible for P hase I ESAs for 26 cellular telephone sites in Montana and Wyoming and numerous commercial properties in Montana. (1994)

Expert Witness

• Hydrogeologic and Environmen tal Litigation, Montana. Expert Witness during hearings to determine oil pipeline right-of-way condemnation and property damages due to groundwater impacts from a petrochemical disposal site. (1998)Paul E. Lemire

Tetra Tech Page 3 Petroleum Release Investigations and Corrective Actions

• Fuel Release Investigation and Remediation, Rail Yards, Montana and Washington . Project Manager/ Senior Hydrogeologist responsible for a site investigation and remediation efforts at two rail yards in Montana. Installed numerous monitor we lls, oil recovery wells, Responsible for site characterization, hydrogeologic invest igations, fuel recovery, river s ediment investigation, and soil and groundwater remedial design at two Montana and two Wa shington railroad fueling facilities. Responsible for negotiations with the supervisory agencies. (1996)

Regulatory Compliance

• Regulation of Hazardous Waste Facilities, Montana. As Environmental Specialist, regulated hazardous waste facilities using state and federal RCRA and CERCLA rules for Montana Department of Environmental Quality. (1995)

Risk Assessment

• Oil Refinery RCRA Closure, Permi tting and Investigation, Montana. Project Manager responsible for RCRA facility closure, permitting of land treatment facilities and investigation of RCRA solid waste management units at a Montana oil refinery. (1995)

Fisheries Studies / Management

• Fisheries Studies, Montana . Hydrogeologist responsible for conducting fisheries studies for Montana Department of Fish, Wildlife and Parks. (1976 to 1979)

PROFESSSIONAL AFFILIATONS National Ground Water Association, Member

CONTINUING EDUCATION 40-hr OSHA HAZWOPER, 1986 8-hr OSHA HAZWOPER Refresher, March 2006 Comprehensive First Aid/First Response Training, 2004 Dense Non-aqueous Phase Liqui ds Fate and Transport, 1995 Groundwater Modeling, 1993

PROFESSIONAL EMPLOYMENT HISTORY Senior Hydrogeologist/ Project Scient ist, Tetra Tech, 1999 to Present Senior Hydrogeologist, Environmental Te chnologies & Solutions, Inc., 1996 to 1998 Senior Hydrogeologist, Remediation Technologies, Inc.. 1988 to 1996 Senior Hydrogeologist, Lambi er-Stevenson Engineers, 1988 Hydrogeologist, Remediation Technologies, Inc., 1987 to 1988 Hydrogeologist, Montana Department of Health and Environmental Sciences, 1985 to 1987 Hydrogeologist, Montana Department of Natura l Resources and Conservation, 1982 to 1985 Fisheries Biologist, Montana Department of Fish and Game, 1976 to 1979Tetra Tech Page 1 

## MICHAEL SHANE EWERT

Environmental Technician

EDUCATION Associate of Science in Architectu ral Drafting, DIT – Denver, CO 1996 1 year general studies, MSUB – Billings, MT 1993-94 1.5 years general engineering, MSU – Bozeman, MT 1991-92

REGISTRATIONS/CERTIFICATIONS Concrete Field Testing Technici an, Grade I: (#01090084, Exp. 11/10/11) Safe Operation of Nuclear Soil Mo isture-Density Gauges: MT (12/18/06)

EXPERIENCE SUMMARY Mr. Ewert has 2.5 years of professional experience as an Environmental Technician and over 5 years in the environmental field. He is responsible for all phases of environmental sampling and field characterization for groundwater, surface water, and soils. Handling and shipping field samples for analysis, calibrating and maintaining field equipment, design and installation of product recovery and groundwater remediation systems are also some of his common tasks and res ponsibilities. Mr. Ewert also has an extensive background in various types of construction and provi des oversight and inspection on civil, geotechnical, and environmental projects.

PROJECT EXPERIENCE Computer Aided Drafting

 Various remediation systems, Denver, Colorado. As environmental drafting manager and draftsperson, prepared CAD drawings and design a ssistance on various Soil Vapor Extraction and Air Sparge Systems, architectural plans, architectural and structural detailing, mechanical and electrical layouts, and civil construction designs. (Summer 1996 thru Spring 2002)

Environmental Science

 Lockwood Solvent Groundwater Plume Site, MDEQ, Lockwood, Montana. As environmental field technician, conduct tap water, surface water, and groundwater sampling, including waste water management. (Spring 2007)

 GWIS shutdown quarterly water monitoring, ConocoPhillips Company, Billings, Montana. As environmental field technician, conduct water leve ls, and groundwater sampling, sample handling, and sample shipping. (quarterly, 2006 to present)

 Low/High water Semi-annual water monitoring, ConocoPhillips Company, Billings, Montana. As environmental field technician, conduct water leve ls, and groundwater sampling, sample handling, and sample shipping. (Semi-annual, 2006 to present)

 Semi-annual groundwater monitoring, Cenex Harvest States, Laurel, Montana. As environmental field technician, conduct water levels, and groundw ater sampling and sample handling. (Semi-annual, 2006 to present)

 Quarterly groundwater monitoring, W estern Sugar, Billings, Montana. As environmental field technician, conduct water levels, and groundwater sampling and sample handling. (Semi-annual, 2006 to present)

 Quarterly groundwater monitoring, Billings Landfill, Billings, Montana. As environmental field technician, conduct water levels, and groundwater sampling and sample handling. (Semi-annual, 2006 to present)

 SOSP Remediation and Reuse Project, ConocoPhillips Company Refinery. As environmental technician, excavation oversight of RCRA regulated South Oily Sludge Pits site, material field screening and handling. (July 2008 to November 2008)Michael Shane Ewert

Tetra Tech Page 2 Industrial Hygiene

 Coal Dust Monitoring, PPL Montana, Colstrip, Montana. As environmental technician, conduct exposure monitoring for lead and hexavalent chromi um. (Various turnarounds – 2006 to present)

 Troy Asbestos Property Evaluations, EPA / MT DEQ, Troy, Montana. As environmental technician, inspect and sample local properties for presence of asbestos containing vermiculite. (April 2007 to August 2007)

CONTINUING EDUCATION Hazardous Waste Operations and Emergency Response, August 2006 8-hour HAZWOPER Refresher, March 2008 DOT Hazardous Materials Transportation Online Course, October 2008 Contractor Safety Training Or ientation Program, October 2008 OSHA Asbestos Awareness Training, August 2008 AHA CPR, March 2008

PROFESSIONAL EMPLOYMENT HISTORY Environmental Technician, Tetra Tech, 2006 to present Leadman, JTL Construction, 2004 to 2006 Sales Manager, United Rentals HT, 2002 to 2004 Architectural Sales, Tri-Jack Arch itectural Design Products, 1998 to 2002 Environmental Drafting Manager, Terra con Environmental Inc., 1996 to 1998Tetra Tech Page 1 MICHAEL J. CONNOLLY Environmental Technician

EDUCATION AD, Drafting, Butte Vocational-Technical Center, 1993 Drafting Certificate, Butte Vocational-Technical Center, 1984

REGISTRATIONS/CERTIFICATIONS Underground Storage Tank Remover: Montana (R-0104-172, 2004) Mine Safety and Health Administration Certifi ed Instructor for First Aid Courses (1994)

EXPERIENCE SUMMARY Mr. Connolly has over 15 years of experience as an environmental technician. He performs Phase I site investigations and is responsible for all phases of environmental sampling and field characterization for groundwater, surface water, and soils. He also labels and ships field samples for lab analysis and calibrates, maintains, and repairs field equipment. He performs site design and installs, operates, and maintains soil vapor extraction, product recovery, pump-and-treatment remediation, and chemical injection systems for temporary and permanent site conditions. Mr. Connolly also provides drafti ng support and construction inspection and job oversight for municipal, geotechnica l, and environmental projects. He has extensive experience in various levels of personal protective equipment.

PROJECT EXPERIENCE Bioterrorism Response

 Anthrax Contamination Emergency Response, Capitol Hill, Washington DC. Emergency Response Team Member assisting the US Environmental Prot ection Agency with biological sampling of anthrax found in the Hart Senate Office Building and Senate Mail Processing Facility. Managed multiple sampling, oversight, reconnaissance and remediation teams in the Hart building during both the anthrax and chlorine dioxide gassing events where wipe, swab, and high efficiency particulate air vacuum sampling for anthrax contamination was conducted in several office s. Ensured proper technique for sample collection, managed collected samples, decontaminated sample c ontainers and maintained proper chain-of-custody for collected samples. (2002)

Industrial Hygiene

 Exposure Monitoring near Potentially Radioactive Material, Idaho. Environmental Technician responsible for conducting exposure monitoring during volatile organic compound and groundwater sampling activities and during soil removal and containment activities of potentially radioactive material. Conducted industrial hygiene noise measurement; heat stress monitoring; personal sampling for air contaminants using dragger tubes and SKC samp ling pumps; dust, mist and fume screening; and continuous air sampling with a photo-ionization detector meter for volatile organics. (1993)

 Weather Surveillance, Idaho National Engineering and Environmental Laboratory Projects, Idaho. Environmental Technician responsible for conduc ting weather surveillance, including wind speed and lightning monitoring. (1994)

 Exposure Monitoring, Hydrocarbon Release Sites, Montana . As Environmental Technician, conduct exposure monitoring during excavation and insta llation of water and sewer lines through known hydrocarbon release sites. Screen soil during remova l of known contaminated materials and ensure that sampling, containment and disposal activities are properly reported and completed per local, state and federal guidelines. Completed numerous projects for the City of Billings. (1992 to present)

 Noise and Audibility Complia nce Monitoring, Montana. As Environmental Technician, field-tested locomotive air horn operations to ensure complianc e with Department of Transportation standards for railroad crossing, locomotive distance and audibility. (1992)

 Exposure Monitoring, Colstrip, Montana. As Environmental Technician, conduct level “B” entry into vaults containing hydrochloric acid . Identify the leaking source area and sample the floor material to facilitate determination of the c oncentration of known material and the type of cleanup operation needed. Provide the client with accurate vault c onfiguration information. (2001 to present)Michael J. Connolly

Tetra Tech Page 2  Personal and Area Exposure Monitoring at Coal Mine, Colstrip, Montana. As Environmental Technician, conducted emergency response exposure m onitoring during turn-around of Colstrip furnace maintenance. Located and identified t he potential source causing workers to feel ill. Conducted area and personnel monitoring of coal dust. (2003, 2005)

Computer Aided Drafting

 Computer-Aided Drafting (CAD) Drawings, Montana, Idaho, and New York. As Drafter, prepared CAD drawings of process flow diagrams, piping and instrumentation drawings, electrical/mechanical drawings, architectural drawings, structural steel s upport and construction drawings, certificates of survey and geological/geophysical maps and contours. (1989, 1997)

Health and Safety

 Emergency Response Courses, Montana and Idaho . As Trainer, provided health and safety training for environmental consulting firms; construction, drilling, chemical and mining companies; and various Montana communities. (1998)

 Health and Safety Services, Billings, Montana. As Health and Safety Coordinator, maintained the continued effectiveness of Tetra Tech’s health and safe ty program. Wrote site-specific health and safety plans, conducted tailgate safety meetings, conducted job site safety inspections, and assisted with monthly safety meetings. (2000)

Emergency Response

 Field Operation Emergency Res ponses, Montana and Wyoming. As Environmental Scientist/ Field Technician, provide initial and continuing response to gasoline/diesel releases of pipelines, refinery processing units, sump/ drain overfills and highway tanker spills. Tasks include over-excavation of spill sites, placement of clean replacement material s, and transportation and disposal of contaminated materials. Projects include a pipeline release along Sevenmile Creek at Glendive, Montana; tanker truck rollovers near Bridger, Montana; tanker rollovers near Riverton, Wyoming: and sump overspills and gas station site spills throughout Montana. (1990 to present)

Environmental Site Assessments

 Environmental Site Assessments, Bureau of Indi an Affairs (BIA), Montana, Wyoming, North Dakota, and South Dakota. As Environmental Scientist/ Field Tec hnician, performed field inspection of BIA-funded school facilities for mercury, PCB, mo ld and radon. Sites include all BIA-funded schools in North Dakota. (2004 to 2005)

Compliance Audits

 Compliance Audits, BIA-Funded Facilities, Montana and Wyoming . As Environmental Scientist/ Field Technician, conducted field audit / inspection of BIA- funded facilities for developm ent of a spill, control and containment program as required by Title 40 Code of Federal Regulations (CFR), Part 112. (2005)

 Compliance Audits, Montana Department of Transportation (MT DOT), Montana. As Environmental Scientist/ Field Technician, conducted field audit / ins pection of MT DOT facilities for development of spill, control and containment program as requi red by Title 40 CFR, Part 112. (2004)

 Compliance Audits, Montana Department of Fish, Wildlife and Parks (FWP), Montana. As Environmental Scientist/ Field Technician, conducted fi eld audit / inspection of all FWP facilities prior to development of an updated hazardous communications plan and chemical inventory as required under Occupational Safety and Health Administra tion (29CFR) Part 910.1200 and 1926.59.Trained FWP personnel in hazardous communications plan and awar eness, use of chemical inventory binders and Access database inventory. (2004 to 2005)Michael J. Connolly

Tetra Tech Page 3 CONTINUING EDUCATION 40-hr OSHA HAZWOPER, 1991 8-hr OSHA HAZWOPER Refresher, March 2007 Emergency Medical Services (EMS) Operations & Planni ng for Weapons of Mass Destruction (WMD) (24-hr), 2002 EMS Basic Concepts for WMD Incidents (8-hr), 2002 WMD/Terrorism Awareness for Emergency Responders (8-hr), 2002

PROFESSIONAL EMPLOYMENT HISTORY Environmental Technician, Tetra Tech, 2000 to Present Environmental Technician/Drafter/Emergenc y Response Trainer, MSE-HKM, 1995 to 2000 Drafter, MSE, Inc., 1990 to 1995 Environmental Technician, MSE, Inc., 1992 to 1995 Drafter, Multi - tech Services Division of MSE, Inc., 1984 to 1985