Sampling and Analysis Plan Quality Assurance Project Plan

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FINAL Sampling and Analysis Plan Quality Assurance Project Plan For Stormwater Management At The Malone Services Company Superfund Site Texas City, Galveston County, Texas CERCLIS No.:TXD980864789 Project Number 25008093 Prepared for: Malone Cooperating Parties For Submittal to the USEPA Prepared by: URS Corporation 9801 Westheimer, Suite 500 Houston, Texas 77042 March 2005 001289

Transcript of Sampling and Analysis Plan Quality Assurance Project Plan

Page 1: Sampling and Analysis Plan Quality Assurance Project Plan

FINAL Sampling and Analysis Plan

Quality Assurance Project Plan For

Stormwater Management

At The

Malone Services Company Superfund Site Texas City, Galveston County, Texas

CERCLIS No.:TXD980864789

Project Number 25008093

Prepared for:

Malone Cooperating Parties For Submittal to the USEPA

Prepared by:

URS Corporation 9801 Westheimer, Suite 500

Houston, Texas 77042 March 2005

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SAMPLING A N D ANALYSIS PLAN

Malone Superfund Sitc

Rcv. 2, November 19,2004

P3ge 1 of 22

SAMPLING AND ANALYSIS PLAN

For

STORMWATER

Malone Cooperating Parties

Malone Superfund Site

CERCLIS No.:TXD980864789

Final

Submitted to:

U.S. Environmental Protection Agency

Region 6

Submitted By:

Malone Cooperating Parties

Texas City, Galveston County, Texas

URS Corporation Project Manager

November 2004

Brenda Basile, &.D. URS Corporation Project Quality Control Manager

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TABLE OF CONTENTS

1.0 INTRODUCTION ............................................................................................................................4

2.0 SITE HISTORY................................................................................................................................4

3.0 SAMPLING LOCATION RATIONALE......................................................................................5

4.0 HEALTH AND SAFETY PLAN ....................................................................................................5

5.0 ANALYTES.......................................................................................................................................6

6.0 SURFACE WATER SAMPLING ..................................................................................................6

6.1.1 Direct Sampling ..................................................................................................................6

6.1.2 Bailer ...................................................................................................................................7

6.1.3 Dip Sampler ........................................................................................................................7

6.1.4 Pump ...................................................................................................................................7

6.2 Sample Packaging and Shipping ............................................................................................8

7.0 DECONTAMINATION...................................................................................................................8

8.0 DOCUMENTATION AND RECORDKEEPING........................................................................8

8.1 Sample Naming.......................................................................................................................8

8.2 Field Logbooks........................................................................................................................9

8.3 Sample Container Labels ........................................................................................................9

8.4 Chain-of-Custody Forms ......................................................................................................10

8.5 Security Seal..........................................................................................................................10

8.6 Sample Shipment Documentation ........................................................................................10

8.7 Sample Shipment ..................................................................................................................10

9.0 QUALITY ASSURANCE/QUALITY CONTROL....................................................................10

LIST OF TABLES

Table 1 List of Analytes

LIST OF FIGURES

Figure 1 Sample Location Map

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Figure 2 Example Sample Label

Figure 3 Example Chain-of-Custody

Figure 4 Example Custody Seal

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1.0 Introduction

This Sampling and Analysis Plan (SAP) describes procedures to be implemented during the surface water sampling program at the Malone Superfund Site. Stormwater retained in ditches, bermed areas, and separators constitutes the majority of surface water at the site. Together with the Quality Assurance Project Plan (QAPP), the SAP will provide policies, project organization, objectives, functional activities, and Quality Assurance/Quality Control (QA/QC) measures intended to achieve the project goals associated with the surface water sampling program.

The objectives of the SAP are to assure that:

• Field methods are conducted in a manner consistent with the U.S. Environmental Protection Agency (USEPA) requirements,

• Field methods are conducted in a consistent manner over the course of investigation activities,

• Data generated during field investigations are usable for their intended purpose, and

• Field activities are conducted in a safe manner and in accordance with Facility safety procedures.

Anticipated activities covered under this SAP include:

• Surface water sampling, and

• Decontamination of sampling equipment.

2.0 Site History

The Malone Service Company, Inc. site (Site) is located in Texas City, Galveston County, Texas, in an industrial and petrochemical area constructed on the shores of Swan Lake/Galveston Bay. Figure 1 depicts the Sample Location Map. The Site is enclosed by a 15-18 foot high berm (except for a gate area) that serves as containment for the site. Stormwater accumulates within containment berms and retaining walls around tanks and process equipment, and within several ponds on the site. Internal ditches or laterals direct uncontained stormwater to a discharge collection sump with a discharge pipe leading to Campbell's Bayou, a part of Swan Lake/Galveston Bay. The discharge pipe is normally closed, utilizing a manual screw-operated flapper valve.

The Malone Services Company Superfund Site (MSC) began operating in 1964 as a reclamation plant for waste oils and chemicals. Physical operations ceased in January 1996, and the site has remained inactive since.

The facility was permitted as a commercial storage, processing and disposal facility, authorized to store and process industrial solid wastes under the Texas Commission on Environmental Quality (TCEQ) Hazardous Waste Permit No. HW-50003 from 1984 to 1997. Liquid hazardous and non-hazardous wastes were disposed of by separation and reuse, or disposed of by means of deep well injection under Injection Well Permit Nos. WDW-73 and WDW-138.

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The Hazardous Waste permit included the following storage/treatment units at various times:

• Various above-ground storage tanks for wastewater or recovered oil;

• Various underground tanks to service a decanning unit (not built as of 1988);

• A hydrocarbon distillation unit;

• American Petroleum Institute (API) separator(s); and

• Various hazardous wastewater filters. The permit authorized the receipt of Class I and Class II industrial solid waste with the exception of wastes containing polychlorinated biphenyls (PCBs), explosives and radioactive or nuclear waste material. The permit additionally authorized the discharge of stormwater runoff. No other wastewater discharge permits have been identified.

The facility is currently inactive; however, waste materials, two API separators, two underground injection wells (only one operational), roll-off bins, a large Freshwater Pond, a large pond containing sludge, numerous tanks containing liquid and sludge, and metal drums inside small buildings were left on the site after the plant was closed.

Stormwater will be sampled, analyzed and discharged to Campbell’s Bayou or sent to the deep well for injection only when necessary to (1) maintain safe access to Site areas, or (2) prevent releases of possibly contaminated stormwater from containment in specified units or the Earthen Impoundment “Sludge Pit”.

3.0 Sampling Location Rationale

During the course of investigation activities, sampling locations will be selected to determine the presence or absence of analytes as listed in Table 1 in surface water. Sampling and monitoring locations are presented on Figure 1.

4.0 Health and Safety Plan

Surface water sampling will be conducted in a manner consistent with Facility safety procedures and applicable Occupational Safety and Health Administration (OSHA) regulations found in 29 CFR Part 1910.120. A site-specific Health and Safety Plan (HASP) will be developed by the Lead Technician/Operator prior to initiation of field sampling activities. Activities to be managed under the HASP include but are not limited to:

• Specifying safety training and monitoring requirements,

• Selection of personal protective clothing and equipment,

• Collection of surface water samples,

• Decontamination of equipment (if applicable), and

• Staging of investigation derived wastes (IDW) (if applicable).

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Subcontractors working under the direction of the Lead Technician/Operator will be required to meet and abide by the contents of the HASP.

5.0 Analytes

A target list of analytes has been established for the project. Investigation activities will be conducted to determine the presence of these chemicals in surface water. The list of analytes was developed by reviewing:

• Current and historical facility process operations,

• A list of standard chemicals associated with refining operations, and

• Groundwater and soil results obtained during previous sampling associated with TCEQ and USEPA investigations.

Table 1 lists the analytes for the surface water (stormwater) sampling program. The samples will be analyzed for volatile organic compounds (VOCs) and semivolatile organic compounds (SVOCs), as well as site-specific metals, oil and grease (O&G), cyanide and chemical oxygen demand (COD).

6.0 Surface Water Sampling

Surface water samples can be collected using one of four methods: direct sampling with container, bailer, dip sampler or pump. The sections below describe the procedures for each method.

6.1.1 Direct Sampling

The direct method may be utilized to collect water samples from the surface directly into the sample bottle. This method is not to be used when contact with high concentrations of contaminants is a concern. Using adequate protective clothing, access the sampling station by appropriate means. When using the direct method, do not use pre-preserved sample bottles as the collection method may dilute the concentration of preservative necessary for proper sample preservation.

1. For shallow stream stations, collect the sample under the water surface while pointing the sample container upstream; the container must be upstream of the collector. Avoid disturbing the substrate. For lakes and other impoundments, collect the sample under the water surface avoiding surface debris and the boat wake.

2. Preserve the sample if appropriate, or use pre-preserved sample bottles. Do not overfill bottles if they are pre-preserved. Label the containers as described in the Documentation and Recordkeeping Section.

3. Bottles can also be used for sample collection. In order to collect a sample below the water surface, place a hand over the opening and drop the bottle below the surface to the desired depth then remove the hand from the opening.

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6.1.2 Bailer

A bailer may be used in most situations where site access is from a boat or structure such as a bridge or pier and the water depth is sufficient to accommodate the bailer.

1. Use a properly decontaminated bailer.

2. Tie twine or a rope to the bailer.

3. Lower the bailer into the surface water.

4. Allow the bailer to fill completely.

5. Remove the bailer from the water. Transfer the sample(s) into suitable, sample containers.

6. Preserve the sample if appropriate, or use pre-preserved sample bottles. Do not overfill bottles if they are pre-preserved. Label the containers as described in the Documentation and Recordkeeping Section.

6.1.3 Dip Sampler

The sampler is a glass beaker or glass wide-mouth bottle attached to an extension pole and is suitable for use when sampling from a structure such as a bridge or pier, and where surface samples are required.

1. Extend the device to the sample location and collect the sample by dipping the sampler into the substance.

2. Retrieve the sampler and transfer the sample to the appropriate sample container.

3. Preserve the sample if appropriate, or use pre-preserved sample bottles. Do not overfill bottles if they are pre-preserved. Label the containers as described in the Documentation and Recordkeeping Section.

6.1.4 Pump

A peristaltic pump may be used in most situations where site access is from a boat, samples from a certain depth, or a sweep of the width of narrow streams is required.

1. Install clean medical-grade silicone tubing in the pump head, as per the manufacturing instructions. Allow sufficient tubing on the discharge side of the pump for filling sample containers but only enough on the suction side for attachment to the intake line.

2. Select the length of suction intake tubing necessary to reach the required depth and attach the tubing to intake side of the pump.

3. Position the suction intake tube to the required depth and begin pumping at a slow flow rate to minimize material agitation.

4. Fill the appropriate sample bottles by allowing pump discharge to flow gently down the side of the bottle with minimal entry turbulence.

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5. Preserve the sample if appropriate, or use pre-preserved sample bottles. Do not overfill bottles if they are pre-preserved. Label the containers as described in the Documentation and Recordkeeping Section.

6. Change both the pump tubing and the suction intake tubing prior to the collection of additional samples.

6.2 Sample Packaging and Shipping

Sample storage temperature should be maintained at 4o C from the time the sample is collected. Proper temperature must be maintained in sample storage coolers both in the field, in storage and during shipment to the contract laboratory. This is best accomplished by insuring that there is a sufficient supply of ice during both sample collection and shipment. The use of ice requires the use of a tightly sealed container or multiple layers of sealed plastic bags to contain the melt water.

After collection and the required preservation are completed, the samples should be securely packed in the shipment coolers. Proper sample shipment packing is the responsibility of the sampler. All containers must be clean and dry when packed. All sample labels must be checked for completeness and legibility.

The sample containers should be packed into the coolers allowing space for cushioning and the necessary ice packs. All glass sample containers must be packed in a protective layer to insulate from shock or inadvertent direct contact with the cold packs. Glass containers should never be in direct contact with either other glass containers or the ice packs.

7.0 Decontamination

Decontamination of all non-disposable/non-dedicated sampling equipment is crucial to prevent potential cross-contamination of both the samples as well as the sampling sites. Non-disposable/non-dedicated equipment, however, is generally reserved for backup duty only.

The usual procedure to be utilized for general equipment decontamination will include a non-ionic metal and phosphorus-free laboratory-grade detergent and hot water wash. This wash procedure will be accomplished by thorough scrubbing, utilizing a suitably sized brush, of all interior and exterior surfaces. All equipment will then be triple-rinsed with tap water followed by a triple rinse of deionized water. All equipment will be decontaminated as soon as possible or practical.

8.0 Documentation and Recordkeeping

The paperwork required for sampling documentation and informational purposes includes the field data sheets, chain-of-custody forms, sample labels, security seals, and split sample acknowledgment/receipt forms as described below.

8.1 Sample Naming

Example sample IDs for use in this project are as follow:

Surface Water Locations

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SW804-03250401 Sample collected from surface water location 804 (SW804) which is the Tank 804 containment area. Sample collected on March 25, 2004 (032504).

Trip Blanks

03250401TB First (01) trip blank (TB) sample collected on March 25, 2004 (032504).

Equipment Rinse Blanks

03250402EB Second (02) equipment blank (EB) sample collected on March 25, 2004 (032504).

Field Duplicates

03250401BD First (01) field duplicate (BD for blind duplicate) sample collected on March 25, 2004 (032504)

8.2 Field Logbooks

Each sampling team will maintain a detailed logbook. The signature of the author and the date of entry, the project name and number and the location will accompany all entries in this log. At the beginning of each sampling day, the designated team member will start the daily log by entering the date and time, the locations to be sampled, weather conditions, field team present and any potential problems. Other information to be entered into the field logbook includes observations of field activity taking place, progress, and any problems, summary of equipment preparation procedures and a description of any equipment problems (including corrective action), reference to SOPs, and explanations of any deviations from the work plan or SOPs. At the end of each phase of the investigation, the Lead Technician/Operator will deliver copies of all logbook pages completed during that phase of the investigation to the Project Manager.

8.3 Sample Container Labels

The sample container label is one of the first links in the paper chain that tracks the sample through the sampling and analytical process. Proper identification of sample containers is necessary. Legible, complete, and securely attached labels must be affixed to each sample container. At a minimum, the label information will contain:

• Sample identification

• Name or initials of collection party

• Date and time of collection

• Site and project identification

• Preservation technique and/or filtration

• Parameters required for analysis (if space permits)

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Labels must remain legible and intact when wet. A waterproof black ball point pen or marker will be used to avoid running or smearing of any label information. If problems develop with wet or excessively soiled labels, a protective layer of clear, wide tape may be applied directly over the label after the data has been completely recorded to preserve the legibility of the label data. Example labels are shown in Figure 2.

8.4 Chain-of-Custody Forms

It is necessary to document, with chain-of-custody forms, the possession of the samples from time of sample collection through delivery and check-in at the contract lab. A chain-of-custody record must accompany each set of samples/coolers. The record should be a multi-copy carbonless form. The sampler/shipper will keep a copy for the necessary files. The forms will be securely affixed to the interior top interior of the cooler and will be signed off with each change of possession. Upon arrival at the contract lab, the final entries will be made on the form. A copy of the completed form will then be returned to the sampler. A typical chain-of-custody form is found in Figure 3. The chain-of-custody form will be completed by the laboratory personnel and then returned with the analytical data package for that sampling event.

8.5 Security Seal

A security seal is an adhesive paper-type seal as shown in Figure 4. The seals are fastened to both the lid and side of the coolers to aid in the detection of unauthorized opening of the coolers prior to arrival at the contract laboratory receiving/check-in department. The data from the seal (serial number, etc.) must be recorded on the field data sheet. Seals are not required if the sample coolers are hand-delivered to the lab by the sampling team and the coolers do not leave the sight of the sampling team.

8.6 Sample Shipment Documentation

The bills of lading or air bills provided by the courier companies all require the same general information to be supplied. This information includes the shipper’s name, address, telephone number, account number, as well as the recipient’s name, address, and telephone number. Additional information includes the billing information and the delivery details such as overnight service, Saturday delivery, and cooler weight and dimensions. All of this data must be ready before the coolers are delivered to, or picked up by the courier.

8.7 Sample Shipment

Sample coolers generally require overnight shipment to the contract laboratory. One member of the sampling/shipping personnel groups involved should be the liaison and be responsible for arranging the sample shipments to alleviate any confusion. As previously discussed, all necessary shipping information must be readily available prior to the time of pickup request.

Special cooler handling measures must be undertaken if either extremely high or low temperatures will be encountered during transit to the contact laboratory. High temperatures will require that more ice packs are included with each cooler in order to maintain the 4o C internal cooler temperature.

9.0 Quality Assurance/Quality Control

QA/QC Samples

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During the course of sampling activities, samples will be collected in the field and analyzed by the laboratory for quality assurance/quality control (QA/QC) purposes. The following QA/QC samples will be collected:

• field duplicates,

• equipment rinse blanks ,

• matrix spike/matrix spike duplicates, and

• trip blanks.

The protocols and frequency for QA/QC sampling are specified in the QAPP.

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Table 1

Analyte List

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Antimony, total 7440-36-0 200.7/200.8 5

Arsenic, total 7440-38-2 200.7/200.8 5

Barium, total 7440-39-3 200.7/200.8 5

Beryllium, total 7440-41-7 200.7/200.8 5

Cadmium, total 7440-43-9 200.7/200.8 1

Chromium (III) (total chromium), total 17440-47-3 200.7/200.8 5

Copper, total 7440-50-8 200.7/200.8 5

Lead, total 7439-92-1 200.7/200.8 5

Manganese, total 7439-96-5 200.7/200.8 5

Nickel, total 7440-02-0 200.7/200.8 5

Selenium, total 7782-49-2 200.7/200.8 5

Silver, total 7440-22-4 200.7/200.8 5

Thallium, total 7791-12-0 200.7/200.8 0.005

Zinc, total 7440-66-6 200.7/200.8 5

Mercury, total 7439-97-6 245.1 0.2

Acetone (2-propanone) 67-64-1 624 10

Acrylonitrile 107-13-1 624 50

Benzene 71-43-2 624 10

Bromodichloromethane 75-27-4 624 5

Bromoform 75-25-2 624 5

Bromomethane 74-83-9 624 5

Carbon disulfide 75-15-0 624 10

Carbon tetrachloride 56-23-5 624 10

Chlorobenzene 108-90-7 624 10

Chloroethane (ethyl chloride) 75-00-3 624 10

Chloroform 67-66-3 624 10

Chloromethane 74-87-3 624 20

Cumene (isopropylbenzene) 98-82-8 624 5

Cyclohexane 110-82-7 624 5

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Dibromo-3-chloropropane, 1,2- 96-12-8 624 5

Dibromochloromethane (chlorodibromomethane) 124-48-1 624 5

Dibromoethane, 1,2- 106-93-4 624 5

Dichlorobenzene, 1,2- 95-50-1 624 10

Dichlorobenzene, 1,3- 541-73-1 624 10

Dichlorobenzene, 1,4- 106-46-7 624 10

Dichlorodifluoromethane 75-71-8 624 5

Dichloroethane, 1,1- 75-34-3 624 10

Dichloroethane, 1,2- 107-06-2 624 10

Dichloroethylene, 1,1- 75-35-4 624 10

Dichloroethylene, cis-1,2- 156-59-2 624 5

Dichloroethylene, trans-1,2 156-60-5 624 10

Dichloropropane, 1,2- 78-87-5 624 10

Dichloropropene, cis 1,3- 10061-01-5 624 10

Dichloropropene, trans 1,3- 10061-02-6 624 10

Ethyl benzene 100-41-4 624 10

Ethylene dibromide (dibromoethane, 1,2- ) 106-93-4 624 5

Hexanone, 2- 591-78-6 624 10

Methyl acetate (acetic acid, methyl ester) 79-20-9 624 5

Methyl cyclohexane 108-87-2 624 5

Methyl ethyl ketone (2-butanone) 78-93-3 624 10

Methyl isobutyl ketone (4-methyl-2-pentanone) 108-10-1 624 10

Methylene chloride (dichloromethane) 75-09-2 624 20

MTBE (methyl tert-butyl ether) 1634-04-4 624 5

Styrene 100-42-5 624 5

Tetrachloroethane, 1,1,2,2- 79-34-5 624 5

Tetrachloroethylene 127-18-4 624 20

Toluene 108-88-3 624 10

Trichloro-1,2,2-trifluoroethane, 1,1,2- 76-13-1 624 5

Trichlorobenzene, 1,2,4- 120-82-1 624 5

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Trichloroethane, 1,1,1- 71-55-6 624 10

Trichloroethane, 1,1,2- 79-00-5 624 10

Trichloroethylene 79-01-6 624 10

Trichlorofluoromethane 75-69-4 624 5

Vinyl chloride 75-01-4 624 10

Xylenes, Total 1330-20-7 624 15

Acenaphthene 83-32-9 625 10

Acenaphthylene 208-96-8 625 10

Acetophenone 98-86-2 625 10

Anthracene 120-12-7 625 10

Benzaldehyde 100-52-7 625 10

Benzo(a)anthracene 56-55-3 625 10

Benzo(a)pyrene 50-32-8 625 10

Benzo(b)fluoranthene 205-99-2 625 10

Benzo(g,h,i)perylene 191-24-2 625 10

Benzo(k)fluoranthene 207-08-9 625 10

Biphenyl, 1,1- 92-52-4 625 10

Bis (2-chloroethoxy) methane 111-91-1 625 10

Bis (2-chloroethyl) ether 111-44-4 625 10

Bis (2-chloroisopropyl) ether (2,2’-oxybis(1-chloropropane)) 108-60-1 625 10

Bis (2-ethylhexyl) phthalate 117-81-7 625 10

Bromophenyl phenylether, 4- 101-55-3 625 10

Butyl benzyl phthalate 85-68-7 625 10

Caprolactam 105-60-2 625 10

Carbazole 86-74-8 625 10

Chloro-3-methylphenol, 4- 59-50-7 625 10

Chloroaniline, p- 106-47-8 625 10

Chloronaphthalene, 2- (chloronaphthalene, beta) 91-58-7 625 10

Chlorophenol, 2- 95-57-8 625 10

Chlorophenyl phenylether, 4- 7005-72-3 625 10

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Chrysene 218-01-9 625 10

Cresol, o- (2-methylphenol) 95-48-7 625 10

Cresol, p- (4-methylphenol) 106-44-5 625 10

Dibenz-a,h-anthracene 53-70-3 625 10

Dibenzofuran 132-64-9 625 10

Dichlorobenzidine, 3,3’- 91-94-1 625 10

Dichlorophenol, 2,4- 120-83-2 625 10

Diethyl phthalate 84-66-2 625 10

Dimethyl phenol, 2,4- 105-67-9 625 10

Dimethylphthalate 131-11-3 625 10

Di-n-butyl phthalate 84-74-2 625 10

Dinitro-2-methylphenol, 4,6- (dinitro-o-cresol, 4, 6-) 534-52-1 625 NA

Dinitrophenol, 2,4- 51-28-5 625 50

Dinitrotoluene, 2,4- 121-14-2 625 10

Dinitrotoluene, 2,6- 606-20-2 625 10

Di-n-octyl phthalate 117-84-0 625 10

Fluoranthene 206-44-0 625 10

Fluorene 86-73-7 625 10

Hexachlorobenzene 118-74-1 625 10

Hexachlorobutadiene 87-68-3 625 10

Hexachlorocyclopentadiene 77-47-4 625 10

Hexachloroethane 67-72-1 625 20

Indeno-1,2,3-cd-pyrene 193-39-5 625 10

Isophorone 78-59-1 625 10

Methylnaphthalene, 2- 91-57-6 625 10

Naphthalene 91-20-3 625 10

Nitroaniline, 2- 88-74-4 625 10

Nitroaniline, 3- 99-09-2 625 10

Nitroaniline, 4- 100-01-6 625 10

Nitrobenzene 98-95-3 625 10

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Nitrophenol, 2- 88-75-5 625 20

Nitrophenol, 4- 100-02-7 625 50

Nitrosodi-n-propylamine, n- 621-64-7 625 10

Nitrosodiphenylamine 86-30-6 625 10

Pentachlorophenol 87-86-5 625 10

Phenanthrene 85-01-8 625 10

Phenol 108-95-2 625 10

Pyrene 129-00-0 625 10

Trichlorophenol, 2,4,5- 95-95-4 625 10

Trichlorophenol, 2,4,6- 88-06-2 625 10

Cyanide 57-12-5 335.3 20

Oil and grease NA 1664 5 mg/L

Chemical Oxygen Demand NA 410.4 5 mg/L

MAL – Minimum Analytical Limit

NA – Not Applicable

Methods for the Chemical Analysis of Water and Wastes, 40 CFR 136

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FIGURES

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STORMWATERDRAINAGESUMP

(400)

(300)

(700)

(802) (804)

(801) (803) (804)

(805)

(001)

(002)(003)

(1200B)

(1200A)

(100)

(PIT)

SOURCE: BASE DRAWING OBTAINED FROM CLIENT AND WAS ORIGINATED BY ENVIRONMENTAL CONSULTING ASSOCIATESAUSTIN, TEXAS. DATED SEPT. 1989.

MALONE SERVICE CO.FAX: (713) 914-8404

9801 Westheimer

Houston, Texas 77042PH: (713) 914-6699

Suite 500

1

SAMPLING LOCATIONSSUPERFUND SITESCALE IN FEET

5002500

- CLOSED SOLID WASTE MANAGEMENT UNIT

- PROPERTY BOUNDARY

L E G E N D

- INJECTION WELL LOCATION

- DRAINAGE DITCHES

- CONCRETE-LINED DRAINAGE

- SPECIFIED STORMWATER SAMPLE

- NON-SPECIFIED STORMWATER SAMPLE

STORMWATER

- SAMPLE INDENTIFICATIONS( )

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Figure 2 Example Sample Label

Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, HCl

Analysis: Volatiles EPA 624

Signature:

Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, HCl

Analysis: Volatiles EPA 624

Signature: Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, HCl

Analysis: Volatiles EPA 624

Signature:

Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C

Analysis: Semivolatiles EPA 625

Signature: Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C

Analysis: Semivolatiles EPA 625

Signature:

Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, HNO3

Analysis: Metals 200.7/200.8/245.1

Signature: Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, HCl

Analysis: Oil and Grease EPA 1664

Signature:

Field ID: SW804-072104

Project ID: Malone Superfund Site Stormwater

Date:

Time:

Matrix/Preservative: Water, 4°C, H2SO4

Analysis: Chemical Oxygen Demand EPA 410.4

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M

alone Superfund Site

Rev. 2, Novem

ber 19, 2004 SA

MP

LIN

G A

ND

AN

AL

YSIS P

LA

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Page 21 of 22

Figure 3 Example C

hain-of-Custody

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Figure 4 Example Custody Seal

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QUALITY ASSURANCE PROJECT PLAN

Malone Superfund Site Rev. 2, Novembcr 19,2004

Page 1 of 32

QUALITY ASSURANCE PROJECT PLAN

for

STORMWATER

Malone Cooperating Parties

Malone Superfund Site

CERCLIS No.:TXD980864789

Final

Submitted to:

U. S. Environmental Protection Agency

Region 6

Submitted By:

Malone Cooperating Parties

Texas City, Galveston County, Texas

/I /-I November 2004

David K. Ramsden, Ph.D. URS Corporation Project Manager

Brenda Basile, p h . ~ URS Corporation Project Quality Control Manager

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TABLE OF CONTENTS

1.0 INTRODUCTION.............................................................................................................................4

2.0 PROJECT DESCRIPTION.............................................................................................................4

3.0 DATA QUALITY OBJECTIVES...................................................................................................4

4.0 PROJECT ORGANIZATION AND RESPONSIBILITY ..........................................................4

5.0 QA/QC FOR SAMPLING PROCEDURES..................................................................................5

5.1 Sample Containers, Preservation and Holding Times............................................................5

5.2 Sample Naming.......................................................................................................................5

5.3 Sample Log..............................................................................................................................6

5.4 Field Logbook .........................................................................................................................7

5.5 QC Samples.............................................................................................................................7

5.5.1 Trip Blanks..........................................................................................................................7

5.5.2 Equipment Blanks...............................................................................................................7

5.5.3 Field Duplicates ..................................................................................................................8

5.5.4 Matrix Spikes/Matrix Spike Duplicates .............................................................................8

6.0 EQUIPMENT DECONTAMINATION.........................................................................................8

7.0 SAMPLE CUSTODY PROCEDURES..........................................................................................9

7.1 Sample Containers and Preservation ......................................................................................9

7.2 Sample Packaging and Shipping.............................................................................................9

7.3 Sample Collection and Handling ............................................................................................9

7.4 Chain of Custody.....................................................................................................................9

8.0 ANALYTICAL PROCEDURES...................................................................................................10

9.0 QUALITY CONTROL ACCEPTANCE CRITERIA ...............................................................11

10.0 SUMMARY DATA PACKAGE ...................................................................................................11

10.1 Completed Chain-of-Custody (C-o-C) Documentation.......................................................11

10.2 Sample Identification Cross-Reference ................................................................................11

10.3 Test Reports for Samples ......................................................................................................11

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10.4 Surrogate Recoveries ............................................................................................................12

10.5 Test Reports or Summary Forms for Laboratory Blank Samples .......................................12

10.6 Test Reports or Summary Forms for Laboratory Control Samples (LCS) .........................12

10.7 Test Reports or Summary Forms for Matrix Spike/Matrix Spike Duplicate Samples (MS/MSD).........................................................................................................................................12

10.8 Test Reports for Laboratory Duplicates ...............................................................................13

10.9 Method Quantitation Limits..................................................................................................13

10.10 Other Problems and Anomalies ............................................................................................13

11.0 SUPPORTING DATA REQUIREMENTS .................................................................................13

12.0 DATA VALIDATION ....................................................................................................................14

13.0 ELECTRONIC DATA DELIVERABLES..................................................................................15

14.0 REPORT PREPARATION ...........................................................................................................15

LIST OF TABLES

Table 1 List of Analytes.....................................................................................................................................17

Table 2 Methods, Containers, Preservatives and Holding Times.....................................................................22

Table 3 Calibration Procedures Summary for Analytical Instruments.............................................................24

Table 4 Quality Control Performance Criteria ...................................................................................................25

Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water .......................................................26

LIST OF FIGURES

Figure 1 Project Organization Chart...................................................................................................................16

APPENDICES

Appendix A EDD Format

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1.0 Introduction

This Quality Assurance Project Plan (QAPP) is written to present policies, project organization, objectives, functional activities, and Quality Assurance/Quality Control (QA/QC) measures intended to achieve the project data quality goals during sampling activities associated with the surface water sampling at the Malone Superfund Site located at Texas City, Texas.

This QAPP is intended to meet U. S. Environmental Protection Agency (USEPA) requirements for ensuring that all work is conducted in accordance with QA/QC protocols and field procedural protocols for environmental measurement data. This QAPP, along with the Sampling and Analysis Plan (SAP) constitutes the Field Sampling Plan (FSP).

The plan has been prepared in general accordance with the U.S. Environmental Protection Agency (EPA) document EPA Requirements for Quality Assurance Project Plans (EPA QA/R-5, March 2001).

2.0 Project Description

Surface water data collected from the facility will be used in the stormwater management program and the remedial investigation. Data of sufficient quality and quantity will be collected so that an informed decision can be made for defining and managing the Surface water plumes. Samples will be collected from surface water and will be analyzed for chemical oxygen demand (COD), oil and grease (O&G), target metals, semivolatile organic compounds (SVOCs), and volatile organic compounds (VOCs). Table 1 lists the analytes for the surface water program.

3.0 Data Quality Objectives

The quality of data required for field samples is definitive. This level provides the highest level of data quality and is used for purposes of risk assessment, and evaluation of remediation alternatives. These analyses require analytical methods with rigorous quality control measures and data validation procedures in accordance with U.S. EPA protocols.

4.0 Project Organization and Responsibility

An organizational chart for the project is shown in Figure 1 and project personnel are listed in Appendix A. Responsibilities for project team members are summarized as follows:

The Project Manager is responsible for the execution of the project, including correspondence with and coordinating activities with USEPA and the Malone Cooperating Parties . The Project Manager will receive and maintain original copies of all hardcopy laboratory deliverables, which will be submitted to him by the Project Data Manager following data validation. The Project Manager will authorize payment of laboratory invoices. The Project Manager will develop the field sampling plan, provide technical support, and provide sampling locations to the Lead Technician/Operator. The Project Manager will also provide technical review of project deliverables.

The Lead Technician/Operator will oversee sample collection and supervise all work in accordance with the Work Plan. The Lead Technician/Operator will report to and maintain frequent contact with the Project Manager to ensure that the Project Manager is updated on project progress at all times. The Lead

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Technician/Operator will be responsible for organizing and coordinating the activities of the subcontractor(s), the field crew, and activities associated with sampling activities. The Lead Technician/Operator is responsible for notifying the Project Data Manager of the number of sample locations in advance of a sample event so the Project Data Manager can order the appropriate number of sample containers and coolers from the analytical laboratory. After samples are collected, the Lead Technician/Operator is responsible for providing the Project Data Manager a copy of the chain of custody form (C-o-C) within one working day of sample delivery to the analytical laboratory. At the end of each phase of the investigation, the Lead Technician/Operator will deliver copies of all logbook pages and sample collection forms completed during that phase of the investigation to the Field Support Coordinator.

The Laboratory Project Manager will oversee performance of all analytical tests conducted as part of the project. The Laboratory Project Manager is responsible for providing the Project Data Manager a confirmation of sample receipt within one working day of sample receipt and for notifying the Project Data Manager of any sample integrity issues (holding time exceedances, C-o-C discrepancies, etc.) promptly when discovered. The confirmation of sample receipt will include the following:

• a copy of the C-o-C form,

• a sample login sheet that summarizes sample IDs, as entered into the laboratory information management system (LIMS), and the analyses requested for each sample,

• a summary of the target analytes to be reported for each analysis requested, and

• a summary of any discrepancies or sample integrity issues noted during sample login.

The Laboratory Project Manager is also responsible for submitting the final data package, including hardcopy deliverable and electronic data deliverable (EDD), within the requested turnaround time. The Laboratory Project Manager will send original invoices to the Project Manager for approval and will send a copy of each invoice to the Project Data Manager for review.

The Project Quality Control (QC) Manager will evaluate if sampling procedures, laboratory analyses, and project documentation conducted as part of the project are in accordance with this QAPP. The Project QC Manager will prepare a Data Useability Summary (DUS) in summarizing the review and validation of the data for all deliverables.

5.0 QA/QC for Sampling Procedures

The procedures described in the following sections will be followed during sampling and analytical activities to provide sample documentation and chain of custody control during all transfers of samples. Further details regarding sampling and analysis procedures are provided in the SAP.

5.1 Sample Containers, Preservation and Holding Times

Table 3 lists analytical methods, containers and holding times applicable to the project.

5.2 Sample Naming

Sample labels will clearly identify the particular sample, and should include the following:

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• Facility name and sample ID

• Time and date sample was taken

• Sample preservation

• Analysis requested.

Example sample IDs for use in this project are as follow:

Surface Water Locations

Surface Water Locations

SW804-03250401 Sample collected from surface water location 804 (SW804) which is the Tank 804 containment area. Sample collected on March 25, 2004 (032504).

Trip Blanks

03250401TB First (01) trip blank (TB) sample collected on March 25, 2004 (032504).

Equipment Rinse Blanks

03250402EB Second (02) equipment blank (EB) sample collected on March 25, 2004 (032504).

Field Duplicates

03250401BD First (01) field duplicate (BD for blind duplicate) sample collected on March 25, 2004 (032504).

5.3 Sample Log

The Lead Technician/Operator, or designated representative, will be responsible for keeping a sample log to record information regarding each sample. The required information will include but is not limited to:

• Project number, Facility location

• Sample location description

• Sample ID

• Depth

• Analyses requested

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• Time, date, sampler name,

• Equipment used to collect the sample

5.4 Field Logbook

Each sampling team will maintain a detailed logbook. The signature of the author and the date of entry, the project name and number and the location will accompany all entries in this log. At the beginning of each sampling day, the designated team member will start the daily log by entering the date and time, the locations to be sampled, weather conditions, field team present and any potential problems. Other information to be entered into the field logbook includes observations of field activity taking place, progress, and any problems, summary of equipment preparation procedures and a description of any equipment problems (including corrective action), reference to SOPs, and explanations of any deviations from the work plan or SOPs. At the end of each phase of the investigation, the Lead Technician/Operator will deliver copies of all logbook pages completed during that phase of the investigation to the Project Manager.

5.5 QC Samples

For each batch of 20 or fewer samples, sufficient QC samples will be collected to ensure that the appropriate QC measures described in the following sections will be attained. QC samples will be handled, preserved, and documented in exactly the same manner as those of the sample batch. To minimize bias in the laboratory, field QC samples will be submitted to the laboratory as blind samples using identification codes in the same form as regular samples but identifiable only by select non-laboratory project staff. QC sample requirements are summarized in Table 4.

5.5.1 Trip Blanks

Trip blanks are prepared prior to the sampling event by the analytical laboratory in the actual sample container using Type II reagent-grade water. Trip blanks are kept with the investigative samples throughout the sampling event. They are then packaged for shipment with the investigative samples and sent for analysis. At no time after their preparation are the sample containers to be opened before they reach the laboratory. Trip blanks are to determine if samples were contaminated during storage and transportation from/to the laboratory. If multiple shipments of samples are required, trip blanks are to be provided per shipment but not per cooler. Trip blanks are analyzed for volatile organic parameters. The number of trip blanks can be reduced if VOC samples are segregated into one cooler.

5.5.2 Equipment Blanks

Equipment blanks are defined as samples that are obtained by running Type II reagent-grade deionized water over/through sample collection equipment after it has been cleaned (i.e., rinse water will be poured from the bailer, pumped through the sample pump and tubing, or poured over the augers). Equipment blanks are only collected from non-dedicated, reusable equipment. Type II reagent-grade deionized water will be obtained from the laboratory or an equivalent from a commercially available source. These samples will be used to determine if decontamination procedures were adequate. (The equipment could have been cleaned in the field or prior to the field operation). One equipment blank will be collected each day

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sampling activities occur or for each day of sampling, whichever is the higher frequency. Equipment blanks are collected for each equipment type. Equipment blanks are analyzed for all parameters associated with the sampling event.

5.5.3 Field Duplicates

Field duplicate samples are two or more samples collected simultaneously in separate containers from the same source under identical conditions. One duplicate sample will be collected for each batch of 20 or fewer field samples. The duplicate sample provides a measure of precision, or reproducibility of the sample result. During data validation, precision as a relative percent difference (RPD) will be calculated according to the following equation:

(R1 – R2) * 200 RPD = (R1 + R2)

Field duplicate samples are analyzed for all parameters associated with the sampling event.

5.5.4 Matrix Spikes/Matrix Spike Duplicates

Matrix spikes provide information about the effect of the sample matrix on the preparation and measurement methodology. All matrix spikes are performed in duplicate and are hereinafter referred to as MS/MSD samples. Sufficient sample volume will be collected (triple the normal sample volume) for at least one sample in each batch of 20 or fewer field samples so that MS/MSD samples can be prepared for analysis. If yield is insufficient to fill three times the normal sample volume, the MS/MSD sample should be collected at another location.

6.0 Equipment Decontamination

All reusable, non-dedicated sample collection apparatus will be fully decontaminated before sampling and between sampling events. Disposable equipment will not have to be decontaminated if the equipment is sealed in the original manufacturer’s packaging. Sampling and measurement equipment will be decontaminated using the following sequence:

• Wash with non-phosphate detergent and tap water

• Rinse with tap water twice

• Rinse with distilled/deionized water

All decontamination water will be collected and containerized in Department of Transportation (DOT) approved containers for disposal into the injection well system.

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7.0 Sample Custody Procedures

7.1 Sample Containers and Preservation

The laboratory will supply sample kits. The sample kits will be packaged in coolers and will include the appropriate sample containers. Decontamination deionized water (Type II reagent-grade) will also be obtained from the laboratory or an equivalent from a commercially available source. Table 3 summarizes sample volumes, container types, preservation requirements and holding times. The pH of water samples will be adjusted in the field, as indicated in Table 3, to preserve the chemical and physical integrity of the sample during transport and storage prior to analysis. The laboratory will supply preservatives as described in Table 3 in sample bottles.

7.2 Sample Packaging and Shipping

Following collection, samples will be packaged tightly in coolers with bubble wrap to prevent breakage or damage. Samples will be shipped to the laboratory via overnight commercial carrier, delivered to the laboratory by a member of the field sampling team, or picked up from the Facility by a laboratory representative. A copy of the C-o-C will be faxed or e-mailed to the Project Data Manager by the Lead Technician/Operator within one working day of sample shipment.

7.3 Sample Collection and Handling

During sample collection, fill sample containers to the preferred volume listed in Table 3. Following sample collection, immediately place the lid on the sample container, wipe the container clean, and affix the completed sample label. Immediately after labeling, place the container in bubble-wrap to protect it from breakage, place the container in an ice-filled cooler, and close the cooler lid. Fill out the C-o-C form, as described in Section 7.4 below, as samples are collected.

7.4 Chain of Custody

C-o-C procedures are intended to maintain and permanently document sample possession from the time of collection to disposal, in accordance with US EPA guidelines. A sample is considered to be under a person's custody if:

• It is in that person's possession

• It is in that person's view, after being in that person's possession

• It was in that person's possession and was locked up by them to prevent tampering

• It has been placed in a designated secure area by that person

The C-o-C record will be initiated in the field for all samples collected. At a minimum, the following information shall be recorded on the form:

• Signature of custodian

• Date of receipt and relinquishment

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• Sample IDs

• Sampling date and time

• Sample type and quantity

• Analyses to be performed

• C-o-C tape number (Note: C-o-C tape is not mandatory if samples are hand-delivered)

• Method of shipment and courier name(s) in the remarks box, if applicable

The initial custodian will sign the C-o-C record; enter the date and time; tear off and file the back copy with the appropriate sampling log; and place the remainder in the shipping container with the samples. The sample documentation will be placed in a sealed plastic bag and taped to the inside lid of the cooler.

The laboratory sample custodian will receive and sign the form for the laboratory, and record the date, time of receipt. The laboratory log-in record will explicitly state the condition of the sample containers, any evidence of damage, preservation, and the completeness of accompanying records. After inspection, each sample will be logged in and assigned a unique laboratory sample ID. In addition, the following information will be entered in the logging system for each sample:

• Field sample ID

• Laboratory sample ID

• Date received

• Project name and number

• Collection date

• Sample type

• Analyses to be performed

After sample log-in is complete, a copy of the C-o-C record, with laboratory sample numbers and notations of any discrepancies, will be sent to the Project Data Manager to be entered into the project file. The original C-o-C form will be filed in the laboratory with the shipper's waybill or airbill attached. The Laboratory Project Manager will report any problems or discrepancies immediately to the Project Data Manager. The Laboratory Project Manager is responsible for faxing or e-mailing to the Project Data Manager a confirmation of sample receipt within one working day of sample receipt.

The original copy of the C-o-C form will be included with the final data package submitted to the Project Data Manager.

8.0 Analytical Procedures

Table 1 lists the analytes and required quantitation limits for analysis of project samples. The contracted laboratory will perform all analytical testing, documentation, and reporting. Specific laboratory operations

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are governed by the laboratory’s Quality Assurance Plan, which controls all laboratory activities from the arrival of samples to the reporting of validated analytical data. Supplemental QC criteria are provided in the individual methods and the laboratory’s Standard Operating Procedures (SOPs) used during the analyses of the samples. The laboratory’s SOPs will be made available for review upon request.

9.0 Quality Control Acceptance Criteria

Tables 4 through 7 summarize project quality control acceptance criteria. Table 4 lists the quality control requirements for field measurement equipment. Table 5 summarizes the calibration SW-846 procedures for laboratory instruments used for sample analyses. Table 6 lists the quality control performance criteria for field and laboratory quality control measurements. Table 7 lists the acceptance criteria for laboratory quality control measures.

10.0 Summary Data Package

The Laboratory Project Manager will provide the summary data package described below to the Project Data Manager within the specified turnaround time. Each summary data package should the reportable data listed below. Instrument printouts, laboratory notebook records, calibration and instrument performance records, and other supporting data are not required as part of the summary data package. This supporting data must be archived by the laboratory for a minimum of five years and made available by the laboratory upon request by the USEPA.

The data package should contain, at a minimum, those items outlined below.

10.1 Completed Chain-of-Custody (C-o-C) Documentation

The data package should include copies of the completed field C-o-C forms and documentation, and should also include forms that the laboratory uses to document sample condition upon receipt.

10.2 Sample Identification Cross-Reference

Sample identification cross-reference information facilitates the correlation of field and laboratory sample IDs as well as the association of field samples with a particular laboratory batch. The data package should include a listing of C-o-C field sample IDs cross-referenced to the associated laboratory sample IDs. The data package should include an easy and unambiguous means of associating a specific QC sample (for example, the laboratory duplicate, the MS/MSD samples, and the laboratory control sample) with specific field samples.

10.3 Test Reports for Samples

Sample test reports provide specific information for each sample regarding analytical results and methods. The data package should include the test reports for all reported data. Analytical results (i.e., detected results and non-detected results) should be adjusted for sample characteristics, laboratory preparations/cleanups, and/or laboratory adjustments. All analyte detections above the analyte method detection limit should be reported.

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Sample test reports should include the analytical method, sample quantitation limits (SQLs) for each analyte, dilution factors, method quantitation limits (MQLs), date of analysis. A specific report format is not required, however all columns shall be unambiguously labeled.

10.4 Surrogate Recoveries

Surrogate recovery data are used to evaluate the precision of the analytical method on a sample specific basis. The data package should include the surrogate data as applicable to the analytical method performed. The surrogate data can be included on the test report for each sample, or can be included on a summary form, provided the surrogate results are clearly and unambiguously linked to the sample from which the results were measured. The surrogate data should include the percent recovery (%R) and the laboratory’s QC limits.

10.5 Test Reports or Summary Forms for Laboratory Blank Samples

Analytical results for laboratory blanks provide a means to evaluate laboratory precision and bias, and other potential contamination and carry-over problems. The data package should include test reports or summary forms for all blank samples (for example, method blanks and preparation blanks) pertinent to sample analyses of interest. Blank sample test reports should contain all of the information (e.g., surrogate data) specified for environmental sample test reports/summary forms. Sample data should not be blank corrected. All analyte detections above the analyte method detection limit should be reported.

10.6 Test Reports or Summary Forms for Laboratory Control Samples (LCS)

The data package should include the LCS test reports or LCS results summary forms. A LCS should be included in every preparation batch and taken through the entire preparation, cleanup, and analysis procedures. At a minimum, the LCS samples should contain all target analytes identified for the project (Table 2) applicable to the analytical method performed.

The LCS test report, or LCS results summary form, should include the amount of each analyte added, the %R of the amount measured relative to the amount added, and QC limits for each analyte in the LCS. If required by the laboratory’s QAP and/or SOPs, the %R and relative percent difference (RPD) data for each analyte in the laboratory control sample duplicate (LCSD) should be reported.

10.7 Test Reports or Summary Forms for Matrix Spike/Matrix Spike Duplicate Samples (MS/MSD)

Matrix spikes and matrix spike duplicate (MS/MSD) samples are spiked and analyzed by the laboratory to facilitate identification of effects of the particular matrix of interest on analytical results, particularly biasing of results. If project samples were spiked as MS/MSD samples, the data package should include the MS/MSD test reports or summary forms. The project MS/MSD samples should be spiked with the project-specified analytes.

The project MS/MSD test reports or results summary forms should include identification of the compounds in the spike solution, the amount of each compound added to the MS and the MSD, the parent sample concentration, the concentration measured in both MS and MSD, the calculated %R and RPD, and the QC

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limits for both %R and RPD. The form should also include the laboratory batch number and the laboratory identification number of the sample spiked.

10.8 Test Reports for Laboratory Duplicates

Laboratory duplicates are generated in the laboratory and analyzed to assess method/laboratory precision in the matrix of concern. If a laboratory duplicate was analyzed, the data package should include the duplicate sample test report summary form. The duplicate sample test report should include the calculated RPD between the sample and the sample duplicate results and the QC limits for the RPD. The test report should also include the laboratory batch number and the identification number of the sample. The data package should include an easy and unambiguous means by which the samples associated with that particular duplicate analysis can be identified.

10.9 Method Quantitation Limits

If the laboratory reports the MQL on the test report, the laboratory should specify on the test report whether the MQL has been adjusted for sample characteristics, preparation/cleanups, and/or analytical adjustments. However, to assist the data user in verifying if the appropriate method was used for the analysis, the laboratory data package should include a copy of the laboratory’s unadjusted MQLs for each method and project analyte and each matrix for which data are reported.

10.10 Other Problems and Anomalies

The laboratory should document and report all observed problems and/or anomalies observed by the laboratory that might have an impact on the quality of the data. The laboratory shall include an explanation for any sample in which the results are nondetect and the SQL is elevated due to dilution.

11.0 Supporting Data Requirements

Supporting data for each data package should be retained by the laboratory for a minimum of five years. Specific reporting formats are not required, however all retained data should be legible and clearly labeled with the type of data and with either the applicable laboratory quality control batch numbers or applicable dates.

The laboratory should retain the following supporting data for each field sample, laboratory blank, LCS/LCSD, MS/MSD and duplicate sample, as appropriate for the analytical method:

• Chromatograms and quantitation reports (chromatographic methods).

• Real-time instrument printouts (non-chromatographic methods).

• Laboratory notebook pages (non-chromatographic methods).

The laboratory should also retain extraction/digestion logs that document initial volumes/weights and final volumes for all field and quality control samples. Logs should identify the preparation method using an EPA method reference number. Quality control samples should be identified on the logs (the laboratory assigned identification that appears on the quality control reports included with the test reports is sufficient).

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The laboratory retain provide instrument performance records as appropriate to the analytical method:

• Bar graph spectrum, chromatogram, instrument performance check summary (GC-MS).

• Mass calibration and resolution documentation (ICP-MS).

The laboratory should retain the following supporting data for initial and continuing calibration verifications as appropriate for the analytical method:

• Initial calibration summary form listing each target analyte, standard identification, the response factor for each target analyte in each standard, average response factor or slope and intercept, and the relative standard deviation (RSD) or correlation coefficient (r).

• Calibration verification summary form listing each target analyte, standard identification, the response factor for each target analyte in the verification standard, the average response factor or slope and intercept from the initial calibration curve, and the percent difference (%D) or percent drift (%D).

• Alternatively, the calibration verification summary may list the true concentration, the found concentration, and the percent recovery.

• Chromatograms and quantitation reports (chromatographic methods).

• Real-time instrument printouts (non-chromatographic methods).

• Laboratory notebook pages (non-chromatographic methods).

The laboratory should retain the following supporting data for metals analyses, as appropriate to the analytical method:

• Interference check sample results.

• Serial dilution results.

• Post-digestate spike results.

• Method of standard addition results.

If the laboratory utilizes internal standard quantitation, a comparison of the internal standard areas to acceptance criteria should be retained.

The laboratory should retain a summary of the most recent MDL studies applicable to the analytical methods requested. The laboratory may utilize a composite MDL report if the laboratory has multiple instruments performing the same analytical method. The highest MDL for each analyte, irrespective of the instrument identification, is reported for the composite MDL. The MDL is not rounded up.

12.0 Data Validation

Data generated under this QAPP will be evaluated and qualified using EPA flagging protocols and/or CLP-specified data quality standards as described in the Contract Laboratory Program National Functional

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Guidelines (CLP NFG) for Inorganic Data Review (July 2002) and the CLP NFG for Organic Data Review (October 1999). All data received from the laboratory will be reviewed.

The Data Usability Summary (DUS) should include an examination of

1. the reportable data;

2. the field notes and data associated with the sampling event(s); and

3. the project objectives.

The Project QC Manager will generate a DUS that contains a review of the deficiencies identified in the data, qualifiers identifying biases and unreliable data, assessments of field and laboratory performance, overall precision and accuracy, representativeness and completeness of the data set. The DUS should provide the following information:

• Samples and analytical parameters reviewed

• Field data reviewed

• QC parameters reviewed

• Review criteria for each QC parameter

• Specific samples and constituents that did not meet criteria and applied qualifiers

• Usability of the data

The DUS will be included in the project final report submitted to the USEPA.

13.0 Electronic Data Deliverables

The Project Data Manager will manage data for the project in a project database. The laboratory will submit the electronic deliverables in the URS EZEDD format, suitable for transfer into the Equis database.

14.0 Report Preparation

The Project Manager will be the technical lead for the preparation of reports summarizing the results of the project. All data to be included in summary tables, figures, and data analyses incorporated into project deliverables will be prepared from the project database.

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Figure 1 Project Organization Chart

Project QC Manager Lead Technician/Operator Laboratory Project Manager

URS Project Manager

PRP Committee

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Antimony, total 7440-36-0 200.7/200.8 5

Arsenic, total 7440-38-2 200.7/200.8 5

Barium, total 7440-39-3 200.7/200.8 5

Beryllium, total 7440-41-7 200.7/200.8 5

Cadmium, total 7440-43-9 200.7/200.8 1

Chromium (III) (total chromium), total 17440-47-3 200.7/200.8 5

Copper, total 7440-50-8 200.7/200.8 5

Lead, total 7439-92-1 200.7/200.8 5

Manganese, total 7439-96-5 200.7/200.8 5

Nickel, total 7440-02-0 200.7/200.8 5

Selenium, total 7782-49-2 200.7/200.8 5

Silver, total 7440-22-4 200.7/200.8 5

Thallium, total 7791-12-0 200.7/200.8 0.005

Zinc, total 7440-66-6 200.7/200.8 5

Mercury, total 7439-97-6 245.1 0.2

Acetone (2-propanone) 67-64-1 624 10

Acrylonitrile 107-13-1 624 50

Benzene 71-43-2 624 10

Bromodichloromethane 75-27-4 624 5

Bromoform 75-25-2 624 5

Bromomethane 74-83-9 624 5

Carbon disulfide 75-15-0 624 10

Carbon tetrachloride 56-23-5 624 10

Chlorobenzene 108-90-7 624 10

Chloroethane (ethyl chloride) 75-00-3 624 10

Chloroform 67-66-3 624 10

Chloromethane 74-87-3 624 20

Cumene (isopropylbenzene) 98-82-8 624 5

Cyclohexane 110-82-7 624 5

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Dibromo-3-chloropropane, 1,2- 96-12-8 624 5

Dibromochloromethane (chlorodibromomethane) 124-48-1 624 5

Dibromoethane, 1,2- 106-93-4 624 5

Dichlorobenzene, 1,2- 95-50-1 624 10

Dichlorobenzene, 1,3- 541-73-1 624 10

Dichlorobenzene, 1,4- 106-46-7 624 10

Dichlorodifluoromethane 75-71-8 624 5

Dichloroethane, 1,1- 75-34-3 624 10

Dichloroethane, 1,2- 107-06-2 624 10

Dichloroethylene, 1,1- 75-35-4 624 10

Dichloroethylene, cis-1,2- 156-59-2 624 5

Dichloroethylene, trans-1,2 156-60-5 624 10

Dichloropropane, 1,2- 78-87-5 624 10

Dichloropropene, cis 1,3- 10061-01-5 624 10

Dichloropropene, trans 1,3- 10061-02-6 624 10

Ethyl benzene 100-41-4 624 10

Ethylene dibromide (dibromoethane, 1,2- ) 106-93-4 624 5

Hexanone, 2- 591-78-6 624 10

Methyl acetate (acetic acid, methyl ester) 79-20-9 624 5

Methyl cyclohexane 108-87-2 624 5

Methyl ethyl ketone (2-butanone) 78-93-3 624 10

Methyl isobutyl ketone (4-methyl-2-pentanone) 108-10-1 624 10

Methylene chloride (dichloromethane) 75-09-2 624 20

MTBE (methyl tert-butyl ether) 1634-04-4 624 5

Styrene 100-42-5 624 5

Tetrachloroethane, 1,1,2,2- 79-34-5 624 5

Tetrachloroethylene 127-18-4 624 20

Toluene 108-88-3 624 10

Trichloro-1,2,2-trifluoroethane, 1,1,2- 76-13-1 624 5

Trichlorobenzene, 1,2,4- 120-82-1 624 5

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Trichloroethane, 1,1,1- 71-55-6 624 10

Trichloroethane, 1,1,2- 79-00-5 624 10

Trichloroethylene 79-01-6 624 10

Trichlorofluoromethane 75-69-4 624 5

Vinyl chloride 75-01-4 624 10

Xylenes, Total 1330-20-7 624 15

Acenaphthene 83-32-9 625 10

Acenaphthylene 208-96-8 625 10

Acetophenone 98-86-2 625 10

Anthracene 120-12-7 625 10

Benzaldehyde 100-52-7 625 10

Benzo(a)anthracene 56-55-3 625 10

Benzo(a)pyrene 50-32-8 625 10

Benzo(b)fluoranthene 205-99-2 625 10

Benzo(g,h,i)perylene 191-24-2 625 10

Benzo(k)fluoranthene 207-08-9 625 10

Biphenyl, 1,1- 92-52-4 625 10

Bis (2-chloroethoxy) methane 111-91-1 625 10

Bis (2-chloroethyl) ether 111-44-4 625 10

Bis (2-chloroisopropyl) ether (2,2’-oxybis(1-chloropropane)) 108-60-1 625 10

Bis (2-ethylhexyl) phthalate 117-81-7 625 10

Bromophenyl phenylether, 4- 101-55-3 625 10

Butyl benzyl phthalate 85-68-7 625 10

Caprolactam 105-60-2 625 10

Carbazole 86-74-8 625 10

Chloro-3-methylphenol, 4- 59-50-7 625 10

Chloroaniline, p- 106-47-8 625 10

Chloronaphthalene, 2- (chloronaphthalene, beta) 91-58-7 625 10

Chlorophenol, 2- 95-57-8 625 10

Chlorophenyl phenylether, 4- 7005-72-3 625 10

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Chrysene 218-01-9 625 10

Cresol, o- (2-methylphenol) 95-48-7 625 10

Cresol, p- (4-methylphenol) 106-44-5 625 10

Dibenz-a,h-anthracene 53-70-3 625 10

Dibenzofuran 132-64-9 625 10

Dichlorobenzidine, 3,3’- 91-94-1 625 10

Dichlorophenol, 2,4- 120-83-2 625 10

Diethyl phthalate 84-66-2 625 10

Dimethyl phenol, 2,4- 105-67-9 625 10

Dimethylphthalate 131-11-3 625 10

Di-n-butyl phthalate 84-74-2 625 10

Dinitro-2-methylphenol, 4,6- (dinitro-o-cresol, 4, 6-) 534-52-1 625 NA

Dinitrophenol, 2,4- 51-28-5 625 50

Dinitrotoluene, 2,4- 121-14-2 625 10

Dinitrotoluene, 2,6- 606-20-2 625 10

Di-n-octyl phthalate 117-84-0 625 10

Fluoranthene 206-44-0 625 10

Fluorene 86-73-7 625 10

Hexachlorobenzene 118-74-1 625 10

Hexachlorobutadiene 87-68-3 625 10

Hexachlorocyclopentadiene 77-47-4 625 10

Hexachloroethane 67-72-1 625 20

Indeno-1,2,3-cd-pyrene 193-39-5 625 10

Isophorone 78-59-1 625 10

Methylnaphthalene, 2- 91-57-6 625 10

Naphthalene 91-20-3 625 10

Nitroaniline, 2- 88-74-4 625 10

Nitroaniline, 3- 99-09-2 625 10

Nitroaniline, 4- 100-01-6 625 10

Nitrobenzene 98-95-3 625 10

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Table 1 List of Analytes

Analyte CAS No. Method MAL (µg/L)

Nitrophenol, 2- 88-75-5 625 20

Nitrophenol, 4- 100-02-7 625 50

Nitrosodi-n-propylamine, n- 621-64-7 625 10

Nitrosodiphenylamine 86-30-6 625 10

Pentachlorophenol 87-86-5 625 10

Phenanthrene 85-01-8 625 10

Phenol 108-95-2 625 10

Pyrene 129-00-0 625 10

Trichlorophenol, 2,4,5- 95-95-4 625 10

Trichlorophenol, 2,4,6- 88-06-2 625 10

Cyanide 57-12-5 335.3 20

Oil and grease NA 1664 5 mg/L

Chemical Oxygen Demand NA 410.4 5 mg/L

MAL – Minimum Analytical Limit

NA – Not Applicable

Methods for the Chemical Analysis of Water and Wastes, 40 CFR 136

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Table 2 Methods, Containers, Preservatives and Holding Times

Parameter Analytical Method

Minimum Volume

Preferred Volume Container Preservative Holding Time

Total Metals 200.7/ 200.8/ 245.1 200 ml 500 ml

One 16-oz narrow-mouth HDPE jar with

Teflon®-lined cap

Cool to 4°C; HNO3 to pH < 2

Hg - 28 days from sample collection; 6 months for

other metals

Semi-volatiles 624 1000 ml 2000 ml Two 32-oz narrow-

mouth glass jars with Teflon®-lined cap

Cool to 4°C

Complete extraction w/in 7 days of sample collection. Analyze w/in 40 days of

extraction.

Volatiles 624 40 ml 120 ml Three 40-mL VOA vials with Teflon®-

lined cap

Cool to 4°C; HCl to pH <2. Fill container

completely

Analyze within 14 days of collection.

Oil and Grease 1664 500 ml 1000 ml Two 32-oz narrow-

mouth glass jars with Teflon®-lined cap

Cool to 4°C; HCl to pH <2. Fill container

completely

Analyze within 28 days of collection.

Cyanide 325.3 250 mL 500 ml One 16-oz narrow-

mouth HDPE jar with Teflon®-lined cap

4ºC, NaOH to pH >12 14 days

Chemical Oxygen Demand (COD)

410.4 100 ml 500 ml One 16-oz narrow-

mouth HDPE jar with Teflon®-lined cap

Cool to 4°C; H2SO4 to pH < 2

Analyze within 28 days of collection.

pH 150.1 100 ml 100 ml One 8oz narrow-

mouth HDPE jar with Teflon®-lined cap

None Analyte immediately on-site

Specific Gravity

ASTM D891-95 (Test

Method A) 1000 ml 1000 ml Graduated Cylinder None Analyte immediately on-

site

a – Methods for the Chemical Analysis of Water and Wastes, EPA/600/4-79-020 (March 1983) 1 If sample jars filled, sufficient sample mass (triple required volume) will be available so that for each batch of 20 or fewer field samples, a matrix spike/matrix spike duplicate pair can be prepared.

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Table 3 Calibration Procedures Summary for Analytical Instruments

Calibration Summary

Parameter Measured

Method Description

Reference Activity Requirements

Volatile Organic Compounds

624 GC/MS, Purge & Trap

MCAWW Instrument Performance Check

Run bromofluorobenzene (BFB) for each 12 hour shift. Must meet ion abundance criteria before calibration, per the method. Adjust tune as needed to meet criteria.

Initial Calibration

Analyze a minimum of five concentrations for each analyte of interest. Minimum RRF (0.30/0.10) criteria must be met for each system performance check compound (SPCC) before any samples are analyzed. Maximum %RSD (30%) criteria must be met for each calibration check before any samples are analyzed. Prepare calibration curve for any compound with a %RSD greater than 15%. Take corrective action when criteria not met.

Continuing Calibration

Verify calibration curve every 12 hours with a check standard. Minimum RRF (0.30/0.10) and maximum %D (≤20%) criteria must be met for SPCCs and CCCs.

Semivolatile Organic Compounds

624 GC/MS MCAWW Instrument Performance Check

Run decafluorotriphenylphosphine (DFTPP) for each 12 hours of operation. Must meet ion abundance criteria listed in the procedure before calibration. Adjust tune as required to meet performance criteria.

Initial Calibration

Analyze a minimum of five concentrations for each analyte of interest. Minimum RRF (≥0.05) and maximum %RSD (≤30%) criteria must be met for the SPCCs and CCCs before any samples are analyzed. A calibration curve must be prepared for any compound for which the %RSD is greater than 15%. Take corrective action when criteria not met.

Continuing Calibration

Verify calibration curve every 12 hours with a check standard Minimum RRF (≥0.05) and maximum %D (≤20%) criteria must be met for the SPCCs and CCCs.

Metals 200.7 ICP 200.8 ICP-MS 245.1 AA

MCAWW Initial Calibration

ICP: a blank and one standard establishes the analytical curve. AA: a blank and five standards establishes the calibration curve. Correlation coefficient (r) must be ≥0.995.

Initial calibration Verification

ICP/AA: Analyze check standard. The %R for each analyte must be 90-110%.

Continuing Calibration Verification

ICP: Analyze calibration verification standard every 10 samples. The %R must be 90-110% of the true value. AA: Analyze calibration verification standard every 10 samples. The %R must be 80-120% of the true value.

Interference Tests

ICP: Analyze interference check standard at the beginning of every analytical run. The %R for each analyte must be 80-120% of the true value. If interferences are suspected, run a dilution test or a post-digestate spike. AA: Perform dilution test OR spike recovery test. The %R for each analyte must be 90-110% of the true value.

1" Methods for the Chemical Analysis of Water and Wastes, EPA/600/4-79-020 (March 1983) %D – Percent difference %R – Percent recovery RRF – Relative response factor %RSD – Percent relative standard deviation ICP – Inductively coupled plasma spectrometer AA – Atomic absorption GC/MS – Gas chromatography/ mass spectrometry

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Table 4 Quality Control Performance Criteria

Audit Parameter

Volatiles Semivolatiles Metals Oil and Grease

Method MCAWW 624 MCAWW 625 MCAWW 200.7/200.8/245.1

MCAWW 1664

MQL See Table 1 See Table 1 See Table 1 See Table 1 Holding Times See Table 2 See Table 2 See Table 2 See Table 2 Equipment Blank

Daily < MQL

Daily < MQL

Daily < MQL

Daily < MQL

Field Duplicate One every 20 samples ≤30 RPD (water)

One every 20 samples ≤30 RPD (water)

One every 20 samples ≤20 RPD (water)

One every 20 samples ≤30 RPD (water)

Trip Blank One per sample shipment < MQL

N/A N/A N/A

Instrument Tune/Calibration

See Table 3 See Table 3 See Table 3 N/A

Method (Laboratory) Blank

One per 12 hour shift < MQL (<5 x MQL for common lab contaminants)

Daily per extraction batch < MQL (<5 x MQL for common lab contaminants)

<MQL; per batch per day <MQL; per batch per day

Instrument Blank N/A N/A One per 10 samples analyzed (calibration blank)

N/A

Surrogate Every sample % Recovery (See Table 5 )

Every sample % Recovery (See Table 5 )

N/A N/A

Matrix Spike One per 20 samples %Recovery (See Table 5 )

One per 20 samples %Recovery (See Table 5 )

One per 20 samples %Recovery (See Table 5 )

One per 20 samples %Recovery (See Table 5 )

Matrix Spike Duplicate

One per 20 samples %Recovery RPD (See Table 5)

One per 20 samples %Recovery RPD (See Table 5)

One per 20 samples %Recovery RPD (See Table 5)

One per 20 samples %Recovery RPD (See Table 5)

Internal Standard Area

Each sample 50-100% of amount in calibration standard; Retention time within ±30 seconds from last calibration

Each sample 50-100% of amount in calibration standard; Retention time within ±30 seconds from last calibration

ICP-MS (200.8) only:

The absolute response of any one internal standard must not deviate more than 60-125% of the original response in the calibration blank.

N/A

Laboratory Control Sample

See Table 5 See Table 5 See Table 5 See Table 5

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Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water

LCS Matrix Spike/Matrix

Spike Duplicate Surrogate Recovery Analyte CAS RN

%R %R RPD %R Wet Chemistry

Chemical Oxygen Demand COD 75-125 75-125 20 NA Cyanide Cyanide 80-120 80-120 20 NA Oil and Grease O&G 78-114 78-114 18 NA

Volatile Organic Compounds Dibromofluoromethane 1868-53-7 NA NA NA 70-130 1,2-Dichloroethane-d4 17060-07-0 NA NA NA 76-114 Toluene-d8 2037-26-5 NA NA NA 88-110 4-Bromofluorobenzene 460-00-4 NA NA NA 86-115 Acetone (2-propanone) 67-64-1 60-140 60-140 30 NA Benzene 71-43-2 60-140 76-127 11 NA Bromodichloromethane 75-27-4 60-140 60-140 30 NA Bromoform 75-25-2 60-140 60-140 30 NA Bromomethane 74-83-9 60-140 60-140 30 NA Carbon disulfide 75-15-0 60-140 60-140 30 NA Carbon tetrachloride 56-23-5 60-140 60-140 30 NA Chlorobenzene 108-90-7 60-140 75-130 13 NA Chloroethane (ethyl chloride) 75-00-3 60-140 60-140 30 NA Chloroform 67-66-3 60-140 60-140 30 NA Chloromethane 74-87-3 60-140 60-140 30 NA Cumene (isopropylbenzene) 98-82-8 60-140 60-140 30 NA Cyclohexane 110-82-7 60-140 60-140 30 NA Dibromo-3-chloropropane, 1,2- 96-12-8 60-140 60-140 30 NA Dibromochloromethane (chlorodibromomethane)

124-48-1 60-140 60-140 30 NA

Dibromoethane, 1,2- 106-93-4 60-140 60-140 30 NA Dichlorobenzene, 1,2- 95-50-1 60-140 60-140 30 NA Dichlorobenzene, 1,3- 541-73-1 60-140 60-140 30 NA Dichlorobenzene, 1,4- 106-46-7 60-140 60-140 30 NA Dichlorodifluoromethane 75-71-8 60-140 60-140 30 NA Dichloroethane, 1,1- 75-34-3 60-140 60-140 30 NA

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Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water

LCS Matrix Spike/Matrix

Spike Duplicate Surrogate Recovery Analyte CAS RN

%R %R RPD %R Dichloroethane, 1,2- 107-06-2 60-140 60-140 30 NA Dichloroethylene, 1,1- 75-35-4 60-140 61-145 14 NA Dichloroethylene, cis-1,2- 156-59-2 60-140 60-140 30 NA Dichloroethylene, trans-1,2 156-60-5 60-140 60-140 30 NA Dichloropropane, 1,2- 78-87-5 60-140 60-140 30 NA Dichloropropene, cis 1,3- 10061-01-5 60-140 60-140 30 NA Dichloropropene, trans 1,3- 10061-02-6 60-140 60-140 30 NA Ethyl benzene 100-41-4 60-140 60-140 30 NA Ethylene dibromide (dibromoethane, 1,2- ) 106-93-4 60-140 60-140 30 NA Hexanone, 2- 591-78-6 60-140 60-140 30 NA Methyl acetate (acetic acid, methyl ester) 79-20-9 60-140 60-140 30 NA Methyl cyclohexane 108-87-2 60-140 60-140 30 NA Methyl ethyl ketone (2-butanone) 78-93-3 60-140 60-140 30 NA Methyl isobutyl ketone (4-methyl-2-pentanone)

108-10-1 60-140 60-140 30 NA

Methylene chloride (dichloromethane) 75-09-2 60-140 60-140 30 NA MTBE (methyl tert-butyl ether) 1634-04-4 60-140 60-140 30 NA Styrene 100-42-5 60-140 60-140 30 NA Tetrachloroethane, 1,1,2,2- 79-34-5 60-140 60-140 30 NA Tetrachloroethylene 127-18-4 60-140 60-140 30 NA Toluene 108-88-3 60-140 76-125 13 NA Trichloro-1,2,2-trifluoroethane, 1,1,2- 76-13-1 60-140 60-140 30 NA Trichlorobenzene, 1,2,4- 120-82-1 60-140 60-140 30 NA Trichloroethane, 1,1,1- 71-55-6 60-140 60-140 30 NA Trichloroethane, 1,1,2- 79-00-5 60-140 60-140 30 NA Trichloroethylene 79-01-6 60-140 71-120 14 NA Trichlorofluoromethane 75-69-4 60-140 60-140 30 NA Vinyl chloride 75-01-4 60-140 60-140 30 NA Xylenes, Total 1330-20-7 60-140 60-140 30 NA

Semivolatile Organic Compounds

Nitrobenzene-d5 4165-60-0 NA NA NA 35-114

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Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water

LCS Matrix Spike/Matrix

Spike Duplicate Surrogate Recovery Analyte CAS RN

%R %R RPD %R

2-Fluorobiphenyl 321-60-8 NA NA NA 43-116

Terphenyl-d14 1718-51-0 NA NA NA 33-141

Phenol-d6 13127-88-3 NA NA NA 10-110

2-Fluorophenol 367-12-4 NA NA NA 21-110

2,4,6-Tribromophenol 118-79-6 NA NA NA 10-123

Acenaphthene 83-32-9 60-140 46-118 31 NA Acenaphthylene 208-96-8 60-140 60-140 30 NA Acetophenone 98-86-2 60-140 60-140 30 NA Anthracene 120-12-7 60-140 60-140 30 NA Benzaldehyde 100-52-7 60-140 60-140 30 NA Benzo(a)anthracene 56-55-3 60-140 60-140 30 NA Benzo(a)pyrene 50-32-8 60-140 60-140 30 NA Benzo(b)fluoranthene 205-99-2 60-140 60-140 30 NA Benzo(g,h,i)perylene 191-24-2 60-140 60-140 30 NA Benzo(k)fluoranthene 207-08-9 60-140 60-140 30 NA Biphenyl, 1,1- 92-52-4 60-140 60-140 30 NA Bis (2-chloroethoxy) methane 111-91-1 60-140 60-140 30 NA Bis (2-chloroethyl) ether 111-44-4 60-140 60-140 30 NA Bis (2-chloroisopropyl) ether (2,2’-oxybis(1-chloropropane))

108-60-1 60-140 60-140 30 NA

Bis (2-ethylhexyl) phthalate 117-81-7 60-140 60-140 30 NA Bromophenyl phenylether, 4- 101-55-3 60-140 60-140 30 NA Butyl benzyl phthalate 85-68-7 60-140 60-140 30 NA Caprolactam 105-60-2 60-140 60-140 30 NA Carbazole 86-74-8 60-140 60-140 30 NA Chloro-3-methylphenol, 4- 59-50-7 60-140 23-97 42 NA Chloroaniline, p- 106-47-8 60-140 60-140 30 NA Chloronaphthalene, 2- (chloronaphthalene, beta)

91-58-7 60-140 60-140 30 NA

Chlorophenol, 2- 95-57-8 60-140 27-123 40 NA Chlorophenyl phenylether, 4- 7005-72-3 60-140 60-140 30 NA

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Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water

LCS Matrix Spike/Matrix

Spike Duplicate Surrogate Recovery Analyte CAS RN

%R %R RPD %R Chrysene 218-01-9 60-140 60-140 30 NA Cresol, o- (2-methylphenol) 95-48-7 60-140 60-140 30 NA Cresol, p- (4-methylphenol) 106-44-5 60-140 60-140 30 NA Dibenz-a,h-anthracene 53-70-3 60-140 60-140 30 NA Dibenzofuran 132-64-9 60-140 60-140 30 NA Dichlorobenzidine, 3,3’- 91-94-1 60-140 60-140 30 NA Dichlorophenol, 2,4- 120-83-2 60-140 60-140 30 NA Diethyl phthalate 84-66-2 60-140 60-140 30 NA Dimethyl phenol, 2,4- 105-67-9 60-140 60-140 30 NA Dimethylphthalate 131-11-3 60-140 60-140 30 NA Di-n-butyl phthalate 84-74-2 60-140 60-140 30 NA Dinitro-2-methylphenol, 4,6- (dinitro-o-cresol, 4, 6-)

534-52-1 60-140 60-140 30 NA

Dinitrophenol, 2,4- 51-28-5 60-140 60-140 30 NA Dinitrotoluene, 2,4- 121-14-2 60-140 24-96 38 NA Dinitrotoluene, 2,6- 606-20-2 60-140 60-140 30 NA Di-n-octyl phthalate 117-84-0 60-140 60-140 30 NA Fluoranthene 206-44-0 60-140 60-140 30 NA Fluorene 86-73-7 60-140 60-140 30 NA Hexachlorobenzene 118-74-1 60-140 60-140 30 NA Hexachlorobutadiene 87-68-3 60-140 60-140 30 NA Hexachlorocyclopentadiene 77-47-4 60-140 60-140 30 NA Hexachloroethane 67-72-1 60-140 60-140 30 NA Indeno-1,2,3-cd-pyrene 193-39-5 60-140 60-140 30 NA Isophorone 78-59-1 60-140 60-140 30 NA Methylnaphthalene, 2- 91-57-6 60-140 60-140 30 NA Naphthalene 91-20-3 60-140 60-140 30 NA Nitroaniline, 2- 88-74-4 60-140 60-140 30 NA Nitroaniline, 3- 99-09-2 60-140 60-140 30 NA Nitroaniline, 4- 100-01-6 60-140 60-140 30 NA Nitrobenzene 98-95-3 60-140 60-140 30 NA

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Malone Superfund Site Rev. 1, July 22, 2004 QUALITY ASSURANCE PROJECT PLAN Page 30 of 32

Table 5 LCS, MS/MSD and Surrogate Precision and Accuracy – Water

LCS Matrix Spike/Matrix

Spike Duplicate Surrogate Recovery Analyte CAS RN

%R %R RPD %R Nitrophenol, 2- 88-75-5 60-140 60-140 30 NA Nitrophenol, 4- 100-02-7 60-140 10-80 50 NA Nitrosodi-n-propylamine, n- 621-64-7 60-140 41-116 38 NA Nitrosodiphenylamine 86-30-6 60-140 60-140 30 NA Pentachlorophenol 87-86-5 60-140 9-103 50 NA Phenanthrene 85-01-8 60-140 60-140 30 NA Phenol 108-95-2 60-140 12-110 42 NA Pyrene 129-00-0 60-140 26-127 31 NA Trichlorophenol, 2,4,5- 95-95-4 60-140 60-140 30 NA Trichlorophenol, 2,4,6- 88-06-2 60-140 60-140 30 NA

Metals Antimony 7440-36-0 80-120 75-125 20 NA Arsenic 7440-38-2 80-120 75-125 20 NA Barium 7440-39-3 80-120 75-125 20 NA Beryllium 7440-41-7 80-120 75-125 20 NA Cadmium 7440-43-9 80-120 75-125 20 NA Chromium 7440-47-3 80-120 75-125 20 NA Copper 7440-48-4 80-120 75-125 20 NA Lead 7439-92-1 80-120 75-125 20 NA Manganese 7439-96-5 80-120 75-125 20 NA Mercury 7439-97-6 80-120 75-125 20 NA Nickel 7440-02-0 80-120 75-125 20 NA Selenium 7782-49-2 80-120 75-125 20 NA Silver 7440-22-4 80-120 75-125 20 NA Thallium 7791-12-0 80-120 75-125 20 NA Zinc 7440-66-6 80-120 75-125 20 NA %R - Percent Recovery CAS RN - Chemical Abstracts Service Registry Number LCS - Lab Control Sample NR - Not Required RPD - Relative Percent Difference

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Appendix A

Electronic Data Deliverable Format

- Laboratory EDD File Formats

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URS Standard EDD Format

Rev 1 - May 29, 2002

Electronic data deliverables from the laboratory must be stored in an comma separate variable (CSV) file or an Excel (xls) file using the following standard format. Maximum length of the field is listed under “postion/format” column. If the information is less than the maximum length, do not pad the record with spaces. If EDD is a csv file, each record must be terminated with a carriage return and no final comma. The file can be produced using any software with the capability to create ASCII files. Date is reported as MM/DD/YY or MM/DD/YYYY (month/day/year) and time as HH:MM (hour:minute). Time uses a 24 hour clock, thus 3:30 p.m. will be reported as 15:30. Lab quality control data, such as LCS, method blanks, MS/MSDs, and surrogate data, should not be included.

Column headings Position/format Required/Comments project_name 1 Text20 required sample_id 2 Text20 required as written on COC form sample_date 3 Date required sample_time 4 Time required lab_name 5 Text10 required, keep less than 10 characters lab_sample_id 6 Text20 required, internal lab number lab_anl_method_name 7 Text35 required cas_rn 8 Text15 required, use code if no CAS# exists e.g pH, TOC parameter_name 9 Text60 required, e.g Benzene, pH result_value 10 Text20 required, either the result or "<" followed by the SQL, no extra spaces lab_qualifiers 11 Text7 required if applicable, flags such as U, J, B

result_unit 12 Text15 required, e.g. mg/Kg (use ug instead of µg)

detect_flag 13 Text2 required, put Y if greater than MDL, N otherwise sample_quantitation_limit 14 Text20 required, this is the adjusted MDL dilution_factor 15 Text6 required sample_matrix_code 16 Text10 required, e.g. soil or water

total_or_dissolved 17 Text1 for groundwater metals, "T" for unfiltered, "D" for filtered, "N" if not applicable

basis 18 Text10 required (put "dry", "wet" or "na") analysis_date 19 Date required analysis_time 20 Time required method_detection_limit 21 Text20 provide if possible, otherwise provide in separate table lab_prep_method_name 22 Text35 required if applicable prep_date 23 Date required if applicable prep_time 24 Time required if applicable unadjusted_MQL 25Text20 required client_name 26 Text50 required, e.g URS sample_delivery_group 27 Text10 required, ie. Work order# or lab group # sample_receipt_date 28 Date required sample_receipt_time 29 Time required percent_moisture 30Text5 required, number between 0 and 100 with no "%" sign

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