HERCULES Hercules IncorporatedHercules PlazaWHmington, DE 19894(302) 594-5000Telex; 83-5479

Writer.'s direct dial number:(302) 594-7066

June 27, 1988

Ms. Kate ArthurU . S . Environmental Protection AgencyRegion 61445 ROBS AvenueDallas, Texas 75202-2733Re: Vertac Off-site Areas - Fine Grid Sampling Plan

Jacksonville, ArkansasDear Kate:Transmitted herewith is the Health and Safety Plan (Safety Plan includingdecontamination procedures) for work to be performed under the CERCLAAdministrative Order on Consent for the above-referenced matter. Therevisions you requested after review of a draft of this plan, i . e , theaddition of 2,3,7,8-TCDD to list of chemical hazards and the inclusion of asection on irritating plants under Part 4.0 Emergency Planning, are nowincluded. This Health and Safety Plan is being submitted to EPA for approvalpursuant to paragraph 2 4 . A . of the Order.Also transmitted herewith is the Fish Work Study Plan for Lake Dupree. Thetypographical errors present in the draft version which you reviewed have beencorrected. In addition, as you requested, Section IIB now includes a sentenceconcerning split samples of fish to be provided to EPA. This Fish Work StudyPlan for Lake Dupree is being submitted to EPA for approval pursuant toparagraph 2 4 . 1 . of the CERCLA Administrative Order on Consent for theabove-referenced matter.We look forward to receiving EPA's approval for both of these plans.

Sincerely,

Florence K. fcinosh'ita, Ph.D.Senior lexicologist

Enclosures

cc: Robert E. Hannesschlager, P . E . , ChiefSuperfund Enforcement Branch (6H-E)U . S . EPA, Region 6(with enclosures)BY CERTIFIED MAIL

80700

HEALTH AND SAFETY PLANJACKSONVILLEOFF-SITE SOIL/SEDIMENT SAMPLING

JUNE 23, 1988

1.0 PURPOSE/SCOPE

The objective of this health and safety plan is to assure that safe workingconditions are established and maintained during all operations. This healthand safety plan prescribes the work place procedures which must be followed whenworking with potentially hazardous materials while performing off-site samplingactivities for the Hercules/Vertac project. The safety organization and proce-dures are established based on an analysis of potential hazards. Personnel pro-tection measures will be selected in response to these risks. The requirementsin this plan may change as work progresses due to changing work conditions, butno changes will be made without prior approval of the project safety and healthofficer. The plan is for all IT employees or subcontractors who may be exposedto material believed to be hazardous. Work procedures are meant to comply withOccupational Health and Safety Act (OSHA) requirements of 29 CFR 1910 and thoseof the United States Environmental Protection Agency.

2.0 HAZARD ASSESSMENT ,

Z.I DISCUSSIONAn understanding of the indigenous job site hazards is essential in order todevelop procedures and prescribe equipment necessary to ensure the health andsafety of IT personnel. The chemical and physical hazards described below arethose which will potentially be encountered during off site sampling activities.Management of these hazards will be explained in Sections 3 and 4.

2.2 CHEMICAL HAZARDSThe following hazardous materials are those which have been identified duringprevious environmental sampling surveys:

• Toluene (CAS No. 108-88-3)• 2-chlorophenol (CAS No. 95-57-8)• 4-chlorophenol (CAS No. 106-48-9)

2 3,7,8-TCDD (CAS No. 1746-01-6)2 4-di'chlorophenol (CAS No. 120-83-2)2 6-dichlorophenol (CAS No. 87-65-0)2 3,6-trich1oropheno1 (CAS No. 933-75-5)2 4,6-trichlorophenol (CAS No. 88-06-2)2 4,5-trichlorophenol (CAS No. 95-95-4)2 4-D [(2,4-dich1orophenoxy)acetic acid] (CAS No. 94-75-7)2 4,5-T [(2,4,5-trich1orophenoxy)acetic acid] (CAS No. 93-76-5)Silvex [2-(2,4,5-trich1orophenoxy)propionic acid] (CAS No. 93-72-1)

Additionally, some hazardous chemicals win be used during the decontanii nationof sampling and personal protective equipment. The material used for theseactivities w 1 1 1 be one or more of the fol lowing:

• Hexane• Acetonea Isopropanol• Detergent

2.3 PHYSICAL HAZARDSThe physical hazards to personnel will vary widely depending upon task assign-ments and will often change daily. The following is a summary of those physicalhazards likely to be encountered:

SlipTripFallCutWater/BoatsFireHeat StressSnake BitesDog BitesWork near the police firing rangeExposure to irritating plants

2.4 OXIDATION PONDSSampling activities on the oxidation ponds present unique hazards not only dueto the obvious potential for water or boat mishaps, but also with the potentialfor contact with biological hazards from sewage.

3.0 PROTECTIVE EQUIPMENT/PROCEDURES

3.1 DISCUSSIONOverexposures to site contaminants would have serious consequences but this typeof exposure is implausible given the contaminant concentrations previously foundin the areas to be sampled. This, coupled with the limited level of physicalhazard, warrants only minimal levels of personal protection with responsiblepersonnel conduct.

The primary level of protection w i 1 1 be a modified level D with the exception ofone sampling activity that w i 1 1 require level C.

3.2 S P E C I F I C LEVELS OF P R O T E C T I O N

Activity: Sampling on the oxidation ponds and aeration basinProtective Equipment:

Life VestsPolyethylene Coated Tyvek CoverallsPVC BootiesHalf-Face Respirators with Combination OV/AG and HEPA cartridgesGogglesLatex Gloves

Activity: Soil sampling dry areasProtective Equipment:

• Surgical Gloves

Activity: Soil sampling in wet areasProtective Equipment:

• Surgical Stoves• Boots or Waders• Safety Glasses or Goggles

Activity: Decontamination using solventsProtective Equipment:

• Half-Face Respirator with 0V cartridges• Latex Gloves• Goggles

Act iv i ty : Decontann'nat ion u s i n g detergent or waterProtective E q u i p m e n t :

• Goggles• Latex Gloves

Act iv i ty : S a m p l i n g in marshy , wet, or u n t r a v e l e d areas l i k e l y to harbor poison-ous snakesProtect ive E q u i p m e n t :

• Snake Chaps ( i f waders are not a l ready being w o r n )• Other equ ipmen t ind ica ted by any of the act ivi t ies listed below.

3.3 SAFE WORK PRACTICES

The fol lowing safe work practices will be adhered to by all IT personnel:

• Contamina ted protective e q u i p m e n t , respirators, sampl ingi m p l e m e n t s , waders, etc., sha l l be cleaned or packaged andlabeled pr ior to removal f rom the area where they were used.

• When sampling from a boat, a 1 1 work will be performed by twoperson teams and flotation devices, such as life vests, shallbe worn at all times.

• Legible and understandable precautionary labels shall beaffixed prominently to containers of contaminated equipment,waste, debris or clothing.

• Removal of contaminated soil from protective clothing orequipment by f lowing, shaking, or any other means which dis-perses contaminants into the air is prohibited.

• Employees will wash their face and hands prior to consumingfood or smoking.

• No food w i l l be consumed or tobacco products used d u r i n g workact ivi t ies .

• Flammable solvents will be stored in a well ventilated areaaway from ignition sources.

• W h i l e w o r k i n g i n po ten t ia l ly contaminated areas or thoseknown to have phys ica l hazards , personnel sha l l use the buddysystem ( w o r k i n g i n p a i r s ) . V i s u a l contact sha l l be main-ta ined between crew members d u r i n g such work activit ies.

a Prior to sampling near the gun range, arrangements will bemade with the police so that no shooting wil l take placewhile IT personnel are in the vicinity.

Individuals will observe in others and themselves any indication of adversehealth effects due to chemical or physical agents including:

Changes in complexion and skin discolorationChanges in coordinationChanges in demeanorExcessive salivation and pupillary responseChanges in speech patternHeadachesDizzinessNauseaBlurred VisionCrampsIrritation of eyes, skin, or respiratory tract

4.0 EMERGENCY PLANNING

4.1 I N J U R I E SAll injuries will be reported to the site safety and health officer. Ifnecessary the appropriate IT forms w 1 1 1 be completed in order to comply withOSHA injury reporting requirements.

Injured personnel will be assisted by the first person to encounter them butFirst Aid and CPR will only be provided by trained personnel.

IT will provide and maintain a large industrial first aid kit throughout thisproject.

Employees that require examination and or treatment by a physician will be takento:

Rebsamen Regional Medical Center1400 Braden Road

982-9515

All site personnel will be given directions to the hospital during the first

tailgate safety meeting.

4.2 FIRE EXTINGUISHERSA 10-pound ABC fire extinguisher will be stored in the IT van at all timesthroughout the project.

4.3 HEAT STRESSAH IT personnel will racaive additional training in prevention, detection, andtreatment of heat stress during the first and subsequent tailgate safetymeetings.

Personnel will be al lowed to rest and the work shift adjusted when'necessary toprevent heat stress to personnel. This win be most important during the firsttwo weeks while personnel become acclimated and aware of symptoms.

Gatorade or a similar electroiite replacement beverage win be made available toall personnel throughout the work day.

4.4 SHAKE B I T E S

The most important step is to get the snake bite victim to the hospital quickly. „1—'Meanwhile, take the following first aid measures:

1. Keep the victim from moving around.

2. Keep the victim as calm as possible and preferably in a proneposition.

3. Immobilize the bitten extremity and keep it at or below theheart level.

4. Wi th a hospital dose by, as it is with this project, littleelse is required for first aid. A note of caution: do notmake any cuts or apply a tourniquet/pressure band.

5. If the snake was killed, keep it for identification. Withoutendangering anyone attempt to identify a snake that has notbeen killed.

4.5 DOG/ANIMAL BITES ' -

1. A bit on the face or neck requires special attention.

2. Every effort must be made to restrain any suspected rabidanimal so that it can be kept under observation to determinewhether or not it develops the final stages of rabies. Findout from local health authorities how long a live animal sus-pected of having rabies should be observed.

3. Do not kill the animal unless absolutely necessary. If theanimal has to be killed, have the body examined for rabies.If kill ing is necessary, take precautions not to damage thean imal 's head.

4. If a suspected rabid a n i m a l cannot be caught or found andt h u s cannot be iden t i f i ed and observed, arrange for immediatemedica l care for any person it has bi t ten.

5. In jec t ions are effect ive i n p r e v e n t i n g rabies in 95% of vic-t ims.

5. In the meantime, before the physician takes charge,thoroughly wash the wound with soap and water, flush thebitten area, and apply a dressing.

7. Make sure that the victim avoids movement of the affectedpart until he/she has been attended to by a physician.

4.6 E X P O S U R E TO I R R I T A T I N G PLANTSThese plants include, but are not limited to, poison ivy, oak and sumac. Ofthose who come in direct dermal contact with these plants, 50% may developsevere dermatitis and up to 10% may develop general effects. The following listof information will be used to control this hazard:

1. Personnel shall wear short sleeved shirts, as a minimum, atall times whi le on the job.

2. Site personnel will be educated in the identification ofpoisonous plants during their initial site orientation andsubsequent tailgate safety meetings.

3. Employees shall avoid dermal contact, but when this is notpossible, suitable protective clothing will be utilized.

4. Protective/personal clothing, potentially contaminated byirritating plants, shall be washed with detergent or disposedof on a daily basis.

5. Employees who develop a small amount of skin rash shall betreated with a topical antiseptic and a skin" ointment (thelatter to reduce irritation and itching).

6. Large rash areas or other physical effects w i l l require exam-ina t i on and treatment by a phys ic i an .

7. During various phases of work, irritating plants will havethe highest potential for causing il lness or injury than anyother site hazard. Exposure and irritation should be treatedw i t h the same respect as w o u l d any chemica l /phys ica l agent.

8. Affected employee's condition should be evaluated every fewdays by the site health and safety manager. Treatment by aphysician will be offered to all affected employees.

9. A treatment should be continually carried out for allaffected employee? to prevent opened skin wounds (which are apotential site for chemical exposure) and to maintain on thejob effectiveness.

5.0 TRAINING

All IT employees who work on this project shall have completed a formal trainingprogram and received sufficient field experience to meet or exceed the 40-hourclassroom/3 days on site required by OSHA 1910 .120 . Additionally, all personnelwho are likely to be exposed directly to site contaminants will receive a 1-hourDioxin Hazard Awareness training course. Detailed below are the actual coursetopics covered during the 40 hours of training:

• Basic Safety Training

This course stresses fundamentals such as the cause and pre-vention of slip, trip, and fall hazards, safe drum handlingand opening, safe lifting techniques, heat stress illnessesand their prevention, etc.

• Hazards and Protection

This course deals with the identification, recognition, andsafe work procedures of toxic material. The use and limita-tions of applicable protective clothing, nespirators, anddecontamination procedures are an important part of thiscourse. Respirator fit testing is given to each attendee.

• First Aid and Cardiopulmonary Resuscitation

A large portion of IT personnel will have completed thesestandard Red Cross First Aid and CPR courses.

• 2,3,7,8-TCDD (Dioxin) Hazard Awareness

This course discusses the specific nature of the operationswhich could result in exposure to dioxin, a description ofthe medical surveillance program, the specific protectiveclothing and respirators to be worn on the job. The adversehealth effects associated with exposure to dioxin, the routesof exposure (skin penetration, inhalation, ingestion), andthe safe work procedures associated with the employees jobassignment.

• Other Hazard Awareness

I n f o r m a t i o n w i l l be g i v e n conce rn ing var ious other ma te r i a l sto w h i c h the employee may be exposed. Information willI n c l u d e routes of exposure, toxic effects, appropriate pro-tective e q u i p m e n t , med ica l s u r v e i l l a n c e , and the s p e c i f i cna ture of the job which could result in exposure.

• Health and Safety Programs

H e a l t h and Safety P lans w i l l be discussed in detai l . Infor-mat ion concern ing site engineer ing controls , spec i f ic per-sonal protective equipment , work practices, names of respons-i b l e persons on site, medical s u r v e i l l a n c e requirements , con-t ingency p lans (emergency response) , m o n i t o r i n g of employees, ; . .etc., w i l l be covered.

The f o l l o w i n g t r a i n i n g sessions and in fo rma t iona l mater ia ls w i l l be provided onsite:

• Ta i lga te Safety Meetings

A t a i lga te safety meeting w i l l be conducted at the b e g i n n i n gof each sh i f t , when there is a change i n operat ions , or when-ever a new employee a r r i v e s at the job site once the jobcommences. This meet ing discusses the heal th and safetycons idera t ions for the day ' s ac t iv i t i e s , and outl ines protec-t ive equipment necessary.

6.0 MEDICAL SURVEILLANCE

A11 IT employees on this job shal l have completed a pre-employment medical exam-ina t ion and/or a per iodic update physical examinat ion prior to ass ignment . Theexamina t i on , protocols and parameters comply wi th the requirements of OSHA1910.120. ATI employees w i l l have been cleared by IT 'S examining phys ic ian andcorporate medical department for wear ing nega t ive pressure respirators andocc lus ive c lo th ing .

Al l medical records sha l l be retained in accordance w i t h OSHA Standard 29 CFR1910.20.

The IT medical examina t ion consists of:

• Medica l and Occupat ional His tory Form (de t a i l ed ques t ionna i refor new employees, short ques t ionna i r e for pe r iod ic exams)

• Physica l examina t ion

• Blood analys is

• U r i n a l y s i s

• Chest K-ray

• Pu lmonary Func t ion Test

• A u d i o g r a m

• Electrocardiogram ( i f indicated d u r i n g exam and always foremployees over 40 years of age)

7.0 DECONTAMINATION

Decontamina t ion win be carried out on a l l used protective equipment , s a m p l i n gappara tus , the boat, and any other items wh ich may have become contaminated.Due to the low concentrat ions of site contaminants , personnel decontaminat ionw i l l not be necessary other than f o l l o w i n g good personal hygiene i n c l u d i n gw a s h i n g of hands and face pr ior to eating.

Personal protective equipment ( respirators , etc.) w i l l be cleaned wi th detergenton a routine basis to m a i n t a i n t he i r sanitary condi t ion and to remove potentialchemical con tamina t ion . The boat and a11 protect ive equipment w i l l receive athorough detergent wash before l e a v i n g the site.

S a m p l i n g equ ipment wi11 be decontaminat ion wi th one of three solvents l isted inSection 2.

waste solvents from decontaminat ion that are a l l o w e d to evaporate in an openconta iner w i l l be placed i n a designated area away from ign i t ion sources and theb r e a t h i n g zone of any personnel.

Waste detergent r insate generated from decon tamina t ion win be d is t r ibuted inthe area sampled.

8.0 INFORMATION/DOCUMENTATION

Heal th and Safety Documentat ion w i l l be m a i n t a i n e d in the IT van. Some of thear t ic les a v a i l a b l e for review inc lude :

Medical Examination Reports (clearances)Training RecordsCompleted Tailgate Safety Meeting FormsA Copy of this safety planPaperwork on any accident, injury, or loss that occurred on the project

9.0 ASSIGNMENT OF RESPONSIBILITIES ' .

All personnel will be responsible for continuous adherence to the safety proce-dures during the performance of their assigned tasks. In no case may work be Qperformed in a manner that conflicts with the intent of, or the inherent safetyand environmental cautions expressed in these procedures. Avoiding adversehealth effects and injuries to the site workers is totally dependent on thecontribution of all project participants. The person most responsible for anindividual 's health and safety is the employee himself. A 1 1 IT personnel willbe properly trained in health and safety regulations associated with handlinghazardous materials.

The IT Project Manager, Dana Simerly, will also have the responsibility of thesafety and health officer. These responsibilities include:

• Ensuring compliance of IT personnel with acceptable healthand safety practices including those outlined in this plan.

• Communicating information on changing site conditions to a 1 1IT personnel.

• Conducting Tai lgate Safety Meetings.

• Administration of phases of the health and safety plan.

• Approving any changes or deviance from the plan.• Verif ication of employees credentials to be on the project

(medical, training, etc.).

• Consulting with IT'S health and safety staff when and ifnecessary.

D100X HS

0

FISH WORK STUDY PIAN - LAKE DUPREE

I. OBJECTIVE

The objective of this study plan is to determine the

concentrat ion of 2,3,7,8-tetrachlorodibenzo-p-dioxin

(2 ,3 ,7 ,8 -TCDD) in edible portions of edible fish in Lake

Dupree. In order to meet this objective, fish will be

collected from Lake Dupree. Edible portions, i.e, fillet

minus skin, of representative specimens of collected edible

species will be analyzed for 2,3,7,8-tetrachlorodibenzo-p-

dioxin ( 2 , 3 , 7 , 8 - T C D D ) using high resolution gas

chroinatography/high resolution mass spectrometry

(HRGC/HRMS).

II. SAMPLE COLLECTION

The goal is to collect as many fish as possible. Ideally,

sufficient specimens of size, species and/or feeding habits

will be collected to allow preparation of ten samples for

analyses. Final decisions on actual analyses to be

performed will be based on the number and nature of

specimens collected.

IIA. SAMPLING METHODOLOGY

Fish will be collected by one of two means: electroshocking

and/or the use of gill nets. The method that is most

expedient, while still being approved for use by the

1

Arkansas Gains and Fish Commission, will be used. The fishwill be collected under a scientific collection permitissued by tha Arkansas Game and Fish Commission.

IIB. SAMPU: HANDLING AND DOCUMENTATION

All fish samples will be frozen with the use of dry ice assoon as possible. The specimens will be kept on wet iceuntil each can be properly measured, weighed and tagged witha unique number. A metal tag with the number will be wiredto each specimen to avoid loss of identity. Each specimenwill be wrapped in aluminum foil and placed in a zip-lockbag as appropriate for preservation. The outer packagingwill also be labeled to assist identification. Ice chestssealed with custody tape will be used to ship the samples tothe laboratory.

Split samples will be made available to the EPA projectcoordinator.

Each sample designated for analysis will be analyzed for2,3,7,8-TCDD. All fish samples collected will be classifiedaccording to size, species and/or feeding behavior ( i . e . ,bottom feeders versus predators). If necessary, filletsminus skin of smaller fish of identical species will becomposited. Fillets minus skin portions of larger fish willbe analyzed separately. The specific nature and content of

each analyzed sample will depend on the actual numbers and•types of specimens collected from Lake Dupree.

IIC. FIELD CHAIH-OF-CUSTODY AND RELATED DOCOMEHTATIOH

An essential part of the sampling/analytical scheme is toinsure the integrity of the sample from collection to datareporting. This includes the ability to trace thepossession and handling of samples from the time ofcollection through analysis and final disposal or storage.Routine ITAS sample custody procedures are designed tosatisfy legal requirements tor evidence; samples processedas a part of this program are handled as if each were to bedirectly involved in litigation.

The sample custody procedures in use for this programconform to the guidelines of EPA''s Test Methods forEvaluating Solid Waste (SW-846). The Sampling Coordinatorhas overall responsibility for sample custody in the field.Prior to collecting samples, the Sampling Coordinator issuesnumbered sample tape to the field samplers. Each sample islabeled as it is collected; complete sample documentationconsists of the following:

• A specimen collection form is completed as each sampleis collected. This form contains field sample locationdescriptions and all other pertinent sample informationfor documentation of each sample.

One or more photographs showing the sample and locationis taken, including the best available reference pointsor identification characteristics.A chain-of-custody (C/C) record (Figure 1) is initiatedby the sampling coordinator for each group of tensamples or less in order to track the transfer ofsamples from collection in the field to receipt at thelaboratory. The original of the C/C record mustaccompany the samples at all tines; a copy of each formis maintained in the field for the duration of thesampling effort.A request for analysis (R/A) fora (Figure 2) is alsoinitiated in the field for each group of samplesshipped to the laboratory. The original R/A form mustaccompany the samples to the laboratory, with a copymaintained in the field.

IIIA. ANALYTICAL PROGRAM

All samples will be'analyzed for 2,3,7,8-TCDD at the ITASSpecial Analysis Laboratory (SAL) in Knoxville, Tennessee.Sample preparation and analysis procedures are performedusing modifications of the U . S . EPA Method "Determination of2,3,7,8-TCDD in Soil and Sediment", RCRA Method 8280. Allsamples will be analyzed using high resolution massspectrometry instrumentation to achieve the best possibledetection limits.

A brief description of the analysis procedure intended foreach sample matrix is outlined below. Detailed laboratoryprocedures (SOPs) can be provided on request.

BIOLOGICAL TISSUES (FISH) SAMPLE PREPARATION

In the routine ITAS procedures for preparation of biological4

samples (See Attachment A) , a weighed aliquot of eachmacerated tissue sample and sodium sulfate blank are placedseparate jars, spiked with the internal standard/surrogate mixture and blended with 20g of sodium sulfate.After thorough mixing, 150ml of acetonitrile are added andthe samples are shaken for three ( 3 ) hours on a platformshaker. The resulting extract is filtered into a flask andconcentrated to approximately 1ml. To aid in the removalof chemical interference, samples may be cleaned up usingsilica gel/alumina column chromatography, separatory funneltechniques, or carbon column chromatography. The choice ofclean-up is made according to the complexity of the samplematrix and the severity of interference.

HIGH RESOLUTION GAS CHROMATOGRAPHY/HIGH RESOMTION MASSSPECTROMETRY

The prepared sample extracts are analyzed using HRGC/HRMSscanning in the selected ion monitoring mode for enhancedsensitivity. The column used for isomer-specific analysisis a 60-meter SP-2331 fused silica column. A sample-specific detection limit is calculated as 2.5 times thesignal to noise ratio in the elution window for 2 , 3 , 7 , 8 -TCDD when a "not detected" (MD) is reported. A detectionlimit of ^5 ppt (parts per trillion) is typical for soil andsediment samples (based on a 10 gram aliquot). Forbiological samples, the target detection limit is less than

or equal to 20 ppt,' because of the difficulties associatedwith these matrices, more specific limits cannot beestimated in advance.

IIIB. CALIBRATION PROCEDURES AND FREQUENCYINSTRUMENT PERFORMANCEAt the outset of any 2,3,7,8-TCDD analysis, a performancecheck on the instrument is made to demonstrate compliancewith manufacturer's specifications.

CALIBRATION PROCEDURESFor isomer-specific analyses, a performance mixturecontaining the seven most closely eluting TCDD isomers(including 2,3,7,8-TCDD) is run at the beginning and end ofeach 8 hour shift to demonstrate continuing satisfactoryresolution of the target compound, fn addition, an initialfive-point calibration plot is run in triplicate prior tosample analysis. The mean response factors obtained fromthis initial calibration are used for all subsequentcalculations. The daily calibration standard, analyzed onthe same day as the samples, must produce a response factorwithin 10% of the initial calibration. If the responseobserved from the calibration standard varies by more than10% upon two successive injections, a new calibration curveis established prior to continuing with sample analyses.

IVA. OTTAT.TTY ASSURANCE/QUALITY COHTROL

At all IT Analytical Services facilities, operationalobjectives are directed at providing quality results andservice from the receipt of the sample through the datareport. Data is interpreted by experienced personnel andthoroughly reviewed by the Quality Control Coordinator. Thelaboratory Quality Assurance/Quality Control (QA/QC) planstrives to adhere to the stringent U . S . EPA Dioxin ContractLaboratory Program (CLP) dioxin QA/QC plan. As part of thisprogram, the laboratory has received a 99 out of 100 percentrating on an EPA Performance Evaluation sample analyzed fordioxin in soils. Additionally, IT continues to receive highmarks on Performance Evaluation samples submitted by theU. S . EPA and other regulatory agencies during ongoingprojects as part of the agencies' auditing procedures.

. The data package to be submitted as part of this programwill contain the following items:

Results of the initial calibration including allselected ion current profiles (SICP), as well asresults of calculated response factors of that multi-point .

Completed data reporting sheets with appropriate SICPsand spectra attached. The rounding rules found inSection 7 .2 .2 , "Handbook for Analytical Quality controlin Water and Wastewater Laboratories", EPA 600/4-79-019are applied to all data. Each SICP and Spectrumincludes computer-generated header informationindicating instrumental (GC and MS) operatingparameters during data acquisition.

SICP's generated during each performance check solutionanalysis and each concentration calibration solutionanalysis.A chronological list of all analyses performed. Ifmore than one GC/MS system is used, a chronologicallist is required for each system. The list providesthe sample number, and (if appropriate) the contractorlaboratory sample number for each sample and blank,concentration calibration solution, performance checksolution, including labeled peaks for TCDD isomers, orother pertinent analytical matrix. This list specifiesdate and time analysis was begun. All sample/blankanalyses performed during an 8-hour period areaccompanied by two performance check solution analyses,one preceding and one following sample/blank analyses.If multiple shifts are used, the ending performancecheck sample analysis from one 8-hour period serves asthe beginning analysis for the next 8-hour period.

IVB. LABORATORY QUALITY CONTROL CHECKSOverall effectiveness of a quality control program isdependent upon operation of the laboratory in accordancewith a program which systematically assures the precisionand accuracy of analyses by detecting' errors and preventingtheir recurrence or measuring the degree of error inherentin the methods applied.

The routine internal quality control program includes dailycalibration of instruments using certified standards whenpossible. Glassware is checked tor cleanliness and fordetergent removal prior to each analysis run. Nanogradequality solvents are used for trace organic applications.Each lot of solvent is checked to assure its suitability forthe intended analysis. The highest purity standards

commercially available, usually 98%, are used for

calibration.

To demonstrate that all analytical materials, i.e.,

reagents, glassware and solvents, are free from

interferences, a method blank is assigned to each batch of

15 samples (or less), and is extracted, analyzed and

reported following the identical procedures used for the

accompanying samples.

In accordance with CLP requirements, a matrix spike/matrix

spike duplicate pair will be prepared for each batch of 20

samples (or less). The sample to be spiked and duplicated

will be selected at random by the laboratory at the time the

samples are logged in. Results will be used to demonstrate

the precision and accuracy of the results for these program

samples.

V. SAMPLE TRACKING

Samples arrive at the entrance of the high hazard laboratory

and the shipping container is opened under a hood and

inspected by the Sample Coordinator. Chain-of-custody and

request for analysis forms are signed by the Sample

Coordinator and condition of saniple(s) recorded. (Figure I

and Figure 2)

The Sample Coordinator checks the samples for the followingitems:

• The sample containers are checked for damage such asleaks, spills, broken glass, or unusual odors.Evidence of any damage is reported to laboratorymanagement immediately.

• Sample identification on the sample containers iscompared to that on the Chain-of -Custody.Discrepancies are documented and reported to theLaboratory Manager and QC Coordinator for correctiveaction.

• The custody seals and tapes on sample containers arechecked to ensure that they are intact.

• The number of individual sample containers receivedmust equal the number of samples listed on the Chain-of-Custody or any deviation must be documented andtraceable.

• The Sample Coordinator determines if sufficient volumeof sample for all analyses, QC samples, and potentialretests was supplied.

• The Sample Coordinator fills in "Condition UponReceipt" block of the Chain-of-CUstody form based uponsome criteria for "ok" or not.

• A nonconfonaance memo is completed and given to the QCCoordinator to document any nonconformances and thecorresponding corrective action during sample receipt.

• All samples are handled and stored according to SOPSAL200 "Sample Handling and Storage."

Sample Log In and Project Coding

One sample or a set of samples grouped by a commonreceipt time and common field origin or client areidentified by giving each a laboratory project codecomposed of a unique, client-specific three or fourcharacter code ( e . g . , "EPAL" tor USEPA, Las Vegas) ,

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followed by a five digit number, sequentially assigned,and beginning with 25——.

• Individual samples are assigned sequential 4-digitnumbers preceded by the alphabetic prefix "BB" ( i . e . ,BB2997, BB2998, B B 2 9 9 9 ) , using prenumbered tape.Triplicate labels are affixed to each sample, two ofwhich may be transferred to subsequent aliquots foruse in the laboratory.

• Samples are classified according to matrix type and are : - 'assigned a laboratory reagent blank, in groups of 15 or • - ' .less. Reagent blanks are numbered sequentially; theblank number becomes the batch number. The blank isdesignated by the prefix "BLK" followed by thesequential number ( i . e . , BLK947) ,• this group of samplesthen is designated Batch 947. A matrix spike and Cmatrix spike duplicate are assigned to each batch whenapplicable; they are not applicable in wipe andindustrial hygiene samples, for example. Matrix spikedsamples are denoted by the suffix " M S " ; matrix spikeduplicates by the suffix "MSD" ( i . e . , BB3447MS andBB3447MSD).

Sample information is recorded in the Master Sample Logbook(Figure SAL201-3) by the Sample Coordinator and includes thefollowing:

• Date received• Laboratory sample number• Client sample number• Computer project code tor the LIMS tracking system• Client project name/project code• Sample matrix• Analysis required (method)• Date In/Due• Extraction Page (Batch)/Date• GC/MS Date

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• Report Date• Date Billed

For each batch of samples a sample tracking sheet isgenerated. The Sample Coordinator fills in matrix, sampleID and method. The extraction manager is then notified thatsamples and paperwork are available. All laboratorypersonnel involved with the sample are given a copy of theextraction schedule form.

After the paperwork is filled out, a project file (FigureSAL201-4) is created and the project is entered into theLIMS computer system by the Sample Coordinator.

All original documents (Chain-of -Custody, Request forAnalysis, receiving forms, transportation documents, etc.)are filed in the Field/Client Project File by laboratoryproject number. Paperwork pertinent to sample processing iskept in the laboratory on clipboards for easy access by theanalysts. The analysts are responsible for checking theclipboards at least daily for their test assignments andsample locations.

LABORATORY PROJECT TRACKINGSample analysis and laboratory project status are tracked bythe Master Sample Logbook, LIMS computer system and sampletracking sheets from sample receipt to the issue of the

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report and billing.

Columns are provided in the Master Sample Logbook forrecording the completion date of each stage of theanalysis.Analysts are responsible for completing the portion ofthe sample tracking sheet which is applicable to theirparticular stage of the analysis.

In addition, all projects are listed on the managers'project board indicating date in, due date, number ofsamples, matrix of samples, test(s) to be run, project codeand prices.

VI. PROJECT SCHEDULE

Fish sample collection will begin within 60 days of theeffective date of the order contingent upon approval of thisFish Study Work Plan by EPA. A formal written report will

. be submitted to EPA within 60 days of commencement of fishcollection.

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