Environment International xxx (2014) xxx–xxx

EI-02707; No of Pages 8

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Environment International

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Analysis of environmental contamination resulting from catastrophicincidents: Part 2. Building laboratory capability by selecting anddeveloping analytical methodologies

Matthew Magnuson a,⁎, Romy Campisano a, John Griggs b, Schatzi Fitz-James c, Kathy Hall a, Latisha Mapp d,Marissa Mullins e, Tonya Nichols a, Sanjiv Shah a, Erin Silvestri a, Terry Smith e, Stuart Willison a, Hiba Ernst a

a US Environmental Protection Agency, National Homeland Security Research Center, United Statesb US Environmental Protection Agency, Office of Air and Radiation, National Analytical Radiation Environmental Laboratory, United Statesc US Environmental Protection Agency, Office of SolidWaste and Emergency Response, Office of Resource Conservation and Recovery,Materials Recovery andWasteManagement Division, United Statesd US Environmental Protection Agency, Office of Water, Water Security Division, United Statese US Environmental Protection Agency, Office of Solid Waste and Emergency Response, Office of Emergency Management, CBRN Consequence Management Advisory Team, United States

⁎ Corresponding author.

0160-4120/$ – see front matter. Published by Elsevier Ltdhttp://dx.doi.org/10.1016/j.envint.2014.01.021

Please cite this article as: MagnusonM, et al,oratory capability by selecting..., Environ Int

a b s t r a c t

a r t i c l e i n f o

Article history:Received 1 October 2013Accepted 23 January 2014Available online xxxx

Keywords:Analytical methodsCatastropheInnovationLaboratory analysisLaboratory capacitySustainability

Catastrophic incidents can generate a large number of samples of analytically diverse types, including forensic,clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urbanbuilding and infrastructure materials, and surface residue. Such samples may arise not only from contaminationfrom the incident but also from themultitude of activities surrounding the response to the incident, including de-contamination. This document summarizes a range of activities to help build laboratory capability in preparationfor sample analysis following a catastrophic incident, including selection and development of fit-for-purpose an-alytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are thosewhich have been selected to meet project specific data quality objectives. For example, methods could be fitfor screening contamination in the early phases of investigation of contamination incidents because they arerapid and easily implemented, but those same methods may not be fit for the purpose of remediating the envi-ronment to acceptable levels when a more sensitive method is required. While the exact data quality objectivesdefining fitness-for-purpose can vary with each incident, a governing principle of the method selection and de-velopment process for environmental remediation and recovery is based on achieving high throughput whilemaintaining high quality analytical results. This paper illustrates the result of applying this principle, in theform of a compendium of analytical methods for contaminants of interest. The compendium is based on experi-encewith actual incidents, where appropriate and available. This paper also discusses efforts aimed at adaptationof existing methods to increase fitness-for-purpose and development of innovative methods when necessary.The contaminants of interest are primarily those potentially released through catastrophes resulting frommali-cious activity. However, the same techniques discussed could also have application to catastrophes resulting fromother incidents, such as natural disasters or industrial accidents. Further, the high sample throughput enabled bythe techniques discussed could be employed for conventional environmental studies and compliance monitor-ing, potentially decreasing costs and/or increasing the quantity of data available to decision-makers.

Published by Elsevier Ltd.

1. Introduction

Response to catastrophic incidents involving release of hazardouschemical, biological, and/or radiological contaminants into the environ-ment requires extensive analytical capabilities and capacities. A dis-cussion of what constitutes a catastrophe, along with a detailedintroduction to the use of national laboratory networks to enhanceanalytical capacity following a catastrophic contamination incident,is supplied in Part 1 of this series (Magnuson et al., 2014). Briefly,“capacity” refers to data reporting standards, communication standards,

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Analysis of environmental con(2014), http://dx.doi.org/10.1

and sufficiency of resources tomeet the demand at each stage of remedi-ation and recovery.

Capacity is required because a defining characteristic of catastrophesinvolving release of contaminants is that enormous numbers, potential-ly tens of thousands, of environmental samples are anticipated to be col-lected. Quality analytical results from these samples will be required andexpected in a short period of time. In addition, a significant long termmonitoring effortmay also be necessary,whichwill add to these numbers(DHS, 2004).

Part 1 also summarizes some efforts of the United States Environ-mental Protection Agency (USEPA) to build and ensure national labora-tory capacity for analysis of environmental samples generated fromcatastrophic contamination incidents. USEPA has the primary

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responsibility for both securing water and water infrastructure andremediating indoor and outdoor contamination from a catastrophic in-cident, which can include incidents referred to (in the US) as “Home-land Security” incidents, “incidents of national significance”, and othernames. USEPA established the Environmental Response Laboratory Net-work (ERLN) to assist in the analysis of chemical, biological, and radio-logical samples resulting from catastrophic incidents (USEPA, 2013b).The ERLN integrates capabilities of existing public and private sectorlabs to support environmental responses. ERLN's mission is to provideconsistent analytical capabilities, capacities, and quality data to federal,state, and local decision-makers.

The purpose of this paper is to discuss USEPA technical activitieswith regards to the “capability” for analysis, defined here as the avail-ability of methods, instrumentation, and trained staff. Scientific activi-ties to build this capability fall broadly into two categories: methodselection from existing sources and method development when noappropriate method exists. Because method development can be alengthy and expensive process, selection of analytical methods thatare fit-for-purpose has the potential to advance the timeline of buildinganalytical capability and conserve resources required for method devel-opment. A governing principle of themethod selection and developmentprocess for environmental remediation and recovery is based on achiev-ing high throughput while maintaining high quality analytical results.

2. Selection of analytical methods

After the terrorist and anthrax attacks of 2001, USEPA reviewedthese events and identified several areas to enhance the resiliency ofthe nation following catastrophic incidents related to intentional andunintentional contamination. A critical area identified was the needfor a list of selected analytical methods to be used (ideally) by all labo-ratories when analyzing contamination event samples and, in particu-lar, when analysis of many samples is required over a short period oftime (GPO, 2007; Todd-Whitman, 2002). Utilizing the same set ofmethods can ensure a large available pool of laboratory staff trainedand proficient in a particular set ofmethods and analytical technologies,permits sharing of sample load between laboratories, potentially in-creases the speed of analysis, improves data comparability, and simplifiesthe task of outsourcing analytical support to the commercial laboratorysector. Use of such methods would also improve the follow-up activitiesof validating results, evaluating data and making decisions.

While there could be several approaches to meet this critical needrelated to selection of analyticalmethods before an incident, theUSEPA's“Selected Analytical Methods for Environmental Remediation andRecovery — 2012” (SAM) represents an example which reflects nearlya decade of USEPA's experiences in technical aspects of methodologiesfor the analysis of samples from catastrophic incidents. SAM is the latestupdate of a compendium of methods for use in analyzing samples forchemical, biological, radiological, and biotoxin contamination (USEPA,2012b).

SAM is available as an electronic document, which contains briefsummaries of the methods, including special considerations for theapplication of the method in the context of environmental remediationand recovery. The methods in SAM can also be searched through anonline tool, which provides links to the methods themselves or instruc-tions about how to obtain them. Themethods include detailed laboratoryprocedures for confirming the identification of contaminants and deter-mining their concentrations in environmental samples. The SAMwebsitealso provides separate yet relateddocuments aboutfield screening equip-ment, rapid screening and preliminary identification techniques andmethods, radiological sample collection, and development of radiologicalsample collection plans (USEPA, 2010c). The website also contains adescription and evaluation of “All Hazards Receipt Facility” for conductingan initial evaluation (e.g., triage or screening) of suspected material todetermine if it poses an immediate danger, particularly to laboratory per-sonnel (USEPA, 2010b).

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SAM was developed in support of the ERLN mentioned above;hence, the technical aspects reflected inmethods listed in SAMare coor-dinated with the practical needs of building and ensuring laboratorycapability and capacity. Thus, SAM may provide valuable insights forother laboratories engaged in environmental sample analysis as partof other laboratory networks, even if such networks take a differentform than the ERLN in other countries and regions.

The following discussion highlights some topics that are of particularinterest and importance to the activity of selecting analytical methods,based on the experiences of USEPAwhich includes real-word incidents.The reader is encouraged to keep these topics in mind when perusingthe SAM website. The reader may wish to examine earlier versions ofSAM archived on the website in order to reflect on the evolution ofthese topics.

2.1. Purpose of selected methods

SAM identifies one selected method for each contaminant/sampletype combination tomaximize thefitness of themethod for the purposethat SAM is intended to support: environmental remediation andrecovery. Fit-for-purpose methods are methods that have beenselected to meet project specific data quality objectives (see nextsection). For example, methods used to screen for contamination inthe early phases of investigation of contamination incidents mayhave been chosen because they are rapid and easily implemented, butthose same methods may not be fit for the purpose of remediating theenvironment to acceptable levels when a more sensitive method is re-quired. Aspects that help define what technical features particularmethods should have to make them fit-for-purpose during responseand clearance in a catastrophic incident include: adequate methodthroughput, ability to analyze specific environmental samples, and appro-priate data quality. There aremanynuances in these broad descriptions oftechnical features, and there are many analytical methods that could besuitable for analysis of environmental contaminants (NEMI, 2013).

Methods were selected for SAM to balance these and other consider-ations through a workgroup process composed of experts from federal,state, and local governmental agencies, as well as universities. Separateworkgroups composed of experts with contaminant-specific expertiseprovided input for selection of methods for chemical, biological, biotoxin,and radiological contaminants. Additional details of themethod selectionprocess, including a general decision flowchart, are found elsewhere(USEPA, 2012b).

The methods presented in SAM are designed to be used to:1) determine the extent of site contamination, assuming that earlyresponders have identified contaminants prior to USEPA's remediationeffort; 2) evaluate the efficacy of remediation efforts during site cleanup;and 3) confirm effectiveness of decontamination in support of site clear-ance decisions. While some of the methods compiled in SAM are alsospecified for monitoring of compliance with environmental regulations,the inclusion of a method in SAM does not mean it can be used for com-pliance monitoring of a regulated contaminant. The methods requiredfor such contaminants are usually specified within the regulation itself.The methods in SAM are limited to those that would be used to deter-mine, to the extent possible within analytical limitations; the presenceof chemical, radiological, and biological contaminants of interest; theirconcentrations; and/or viability/harmful activity, when applicable, inenvironmental media.

2.2. Data quality objectives for environmental remediation and recoveryresulting from a catastrophic incident

Data of appropriate quality are required for decisions, but the dataquality objectives are specific to particular incidents and contaminationsites. Consequently, data quality objectives are difficult to generalize,and USEPA has developed and refined detailed processes to ensure ap-propriate data quality for the various types of environmental activities.

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Table 1Sample types (right) for various contaminant types (left) as listed in SAM. A number ofspecific contaminant examples in SAM are listed along-side the contaminant type.

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For more information, the reader is encouraged to visit the vast amountof information and guidance that comprise USEPA's Quality System forEnvironmental Data and Technology (USEPA, 2013c), particularly theguidance documents that detail a systematic process for developingproject specific plans for ensuring the generation of quality data forenvironmental activities (USEPA, 2009). While this guidance coversmany topics and providesmany useful examples for a range of activitiesassociated with catastrophic incidents, it is worthwhile to highlight oneas especially relevant to this discussion: the coordination of large-scaleresponses involving multiple agencies and governmental organizationsthatmay have different approaches and procedures for Quality Systems.Accordingly, it is important to establish a uniform policy for qualityassurance among potential participants in laboratory analysis (DOD/DOE/USEPA, 2005).

In terms of analytical methods for samples from catastrophic con-tamination events, Quality Assurance and Quality Control (QA/QC)need to be designed to assure comparable results between laboratoriesusing the same analytical method and also to allow decision-makersresponsible for site remediation to make consistent decisions based ondata of comparable quality. A perusal of the methods in SAM reveals avariety of levels of detail in QA/QC.

For instance, some prescribe very specific QA/QC and acceptancecriteria, whereas other methods only provide general guidance onQA/QC. SAM does not reconcile differences in the level of QA/QC de-tail because, in practice, site-specific plans are required by USEPA'sQuality System, and those plans should specify appropriate QA/QC forsite-specific goals. Accordingly, the SAM document provides only generalQA/QC guidance (USEPA, 2012a). SAM also defers to guidance fromUSEPA's Forum on Environmental Measurements about ensuring the va-lidity ofmethods of analysis developed for emergency response situations(USEPA, 2010a). While specific to the USEPA's concept of operations, thisdiscussion is intended to illustrate an important point: achieving dataquality during emergency situations can be aided by policy decisionsmade well in advance.

Contaminant types Sample types

Chemicals(142 total)

– Organics– Inorganics– Cyanides– Organometallics– Chemical warfare

agents and degradates

• Solid samples• Aqueous liquid• Drinking water• Air• Wipes

Radiologicals(25 total)

– Alpha emitting– Beta emitting– Gamma emitting– Mixed fission

products– Medical isotopes– Technologically

enhanced naturallyoccurring radiologicalmaterials (TENORM)

– Specific radionuclides– Transuranics

• Drinking water• Aqueous and liquid phase• Soil and sediment• Surface wipes• Air filters• Vegetation

Biologicals(31 total)

– Vegetative bacteria– Spore forming

bacteria– Viruses– Protozoa– Helminths

• Aerosol (growth media,filter, liquid)

• Particulate (swabs,wipes, sponge-sticks,and vacuum socks and filters)

• Drinking water• Post-decontaminationwaste water

Biotoxins (18 total) – Plant toxins– Bacterial toxins– Fungal toxins– Animal toxins– Algal toxins

• Aerosol (filter/cassette,liquid impinger)

• Particulate (swabs, wipes,vacuum socks)

• Solid (soil, powder)• Liquid water (non-potable)• Drinking water

2.3. Contaminants and sample types

Table 1 summarizes the potential contaminants and sample typeslisted in SAM. Among the four contaminant types, biotoxins – toxic sub-stances produced by living organisms – are treated separately from theorganisms that produce them, in part due to differences in the requiredanalytical techniques between the biotoxin and the respective organism.The sample type names correspond to how they are conventionally re-ferred to in many analytical methods, and the sample type names varydepending on contaminant type.

SAM does not contain a complete list of contaminants of interestfrom the standpoint of the analyses needed for all types of catastrophicincidents, nor are all the contaminants in SAM relevant to certain inci-dents. For example, high activity radiological samples and BiosafetyLevel 4 agents (e.g., smallpox virus) are generally only analyzed infew, specialized laboratories, so including methods for these contami-nants would not be consistent with the goals of SAM. Similarly, the listof sample types in SAM could be expanded to be very long. However,the contaminant/sample type combinations contained in SAM are rep-resentative of the range of analytical techniques and methods thatmay be required.

If a laboratory or laboratory network is prepared for the contaminant/sample type combinations in SAM, they are likely to be prepared to dealwith a much larger number of potential contaminant/sample typecombinations. This maymean that they have the equipment, person-nel, and infrastructure which can be applied, perhaps with onlyminor modifications and verifications, to contaminant/sample typecombinations not listed in SAM. For example, for chemical analysis,SAM generically lists “solid samples” to encompass a variety of sam-ple types. Due to potential similarities in sample preparation, similar

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approaches might be used regardless of the solid material requiringanalysis.

2.4. Application of selected analytical methods

Someof the contaminant/sample type combinations listed in SAMcanbe analyzed by methods which are commonly used for other purposes,such as compliance with existing environmental regulations. Where ap-plicable, these methods were selected for SAM. In many cases, there aremultiple methods approved for regulatory compliance which could becandidates for inclusion in SAM. Because the goal of SAM is to select asingle method, the respective workgroups selected, via expert judgment,the most appropriate one for the purpose of SAM.

Many more contaminants are not subject to current environmentalregulation; hence, additional effort is required to apply existing methodsfor analysis of these contaminants. Ideally, appropriate methods existand/or can bemodified to perform the specified analysiswithminimal ef-fort. Otherwise, newmethods could be developed, verified, and validatedto enable the efficient analysis of broad ranges of chemically similar, un-regulated contaminants. Resource and time restrictions require focusingsuch method development efforts on just a few of these contaminantsthat lack environmental regulation. For others, SAM selects the best avail-able method, in case the use of a method for a particular contaminant isrequired before method development activities are completed. SAM isupdated periodically to allow inclusion of any method improvements orto select methods which have emerged since the previous revision.

For those best available methods, it is necessary to convey informa-tion about the appropriate applicability of the method to the user. SAMconveys such information in several ways. First, a summary of eachmethod is supplied within the SAM compendium, which provides

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information about how to perform the method along with some infor-mation about limitations and intent of the method. SAM conveys infor-mation about the applicability of a particular method duringenvironmental remediation. The type of information varies with thecontaminant type in Table 1 (i.e., chemical, biological, radiological, orbiotoxin).

2.4.1. Chemical method applicability considerationsFor chemical contaminants in SAM, the selected methods have been

categorized by “tiers” to indicate a level of method usability for the spe-cific contaminant and sample type. The assigned tiers reflect the conser-vative view for data quality objectives (DQOs) (USEPA, 2009, 2012a)involving timely implementation of methods, analysis of a high numberof samples (such that multiple laboratories are necessary), low limits ofdetection/identification and quantification, and appropriate QC, asshown in Box 1.

Depending on the site-specific data quality objectives, there may beother assignments for the tiers, in addition to the ones which currentlyappear in SAM. Regardless, the goal of the tiers is to provide laboratorieswith an indication of utility of the selected methods among the numberavailable, specifically for the goals of environmental remediation fol-lowing a catastrophic event. The simultaneous use of sound technicaljudgment and technical objectivity is important in assigning thesetiers in order to best serve the data needs of analytical service requestersfor these types of incidents and to help the response community in eval-uating the usefulness of the data.

2.4.2. Biological method applicability considerationsThe biological methods selected for SAM reflect actual biological

incidents, e.g., the anthrax incidents in the United States in 2001,alongwith lessons learned from various biological incidents and trainingexercises since then. Themethods in SAM reflect considerations from theflow diagram (Fig. 1) for sample analysis used in operational response tothese incidents. The pathogenmethods are selected in a response-phaseappropriate manner to facilitate timely and cost-effective analyses.

Box 1Tiers for chemical methods in SAM.

Tier I: Contaminant/sample type is a target of the method(s).Data are available for all aspects of method performance and QCmeasures supporting its use for analysis of environmental samplesfollowing a contamination event. Evaluation and/or use of themethod(s) in multiple laboratories indicate that the methodcan be implemented with no additional modifications for thecontaminant/sample type.

Tier II: (1) The contaminant/sample type is a target of themethod(s) and the method(s) has been evaluated for the contami-nant/sample type by one or more laboratories, or (2) the contami-nant/sample type is not a target of the method(s), but the methodhas been used by laboratories to address the contaminant/sampletype. In either case, available data and/or information indicatethat modifications will likely be needed for use of the method(s)to address the contaminant/sample type.

Tier III: The contaminant/sample type is not a target of themethod(s), and/or no reliable data supporting themethod's fitnessfor its intended use are available. Data from other contaminants orsample types, however, suggest that the method(s), with signifi-cant modification, may be applicable.

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2.4.3. Biotoxin method applicability considerationsWhile the goal of SAM is to identify a single method, it may be very

difficult or impossible tomeet throughput requirements with the appli-cation of only one method for some biotoxins. In this case, SAM recom-mends dividing the samples up into different “analysis types”, with asingle method dedicated to each “analysis type”. For instance, the“analysis type” listed for each biotoxin method in SAM is intendedto address: (1) the level of certainty of results and (2) the remediationphase (e.g., site mapping, assessment, cleanup, clearance).

A sequential approach may be used when assigning the analysistypes, particularly when needed to address a large number of samples.For example, methods identified as “presumptive,”which are generallymore rapid than “confirmatory”methods, might be used during the ini-tial stages of remediation to evaluate the extent of contamination once acontamination event and the type of contamination are known. Pre-sumptive methods also might be used to identify samples that shouldbe analyzed using confirmatorymethods. In turn, the results of the con-firmatory methods might be used to select samples to be analyzed byapplicable “biological activity”methods, which tend to be much slowerand less available than the confirmatory methods. In addition, somebiological activity methods involve the use of animals; therefore, widespread use of such methods when a large number of samples need tobe analyzed may be impractical or impossible due to limitations on thenumber of available animals.

2.4.4. Radiochemical method applicability considerationsThe radiological agents listed in SAM were selected based on the

following considerations: human health impact, radionuclide half-life,environmental persistence, availability of primary radionuclide, poten-tial for dispersion, possible associationwith aweapon detonation, prog-eny radionuclides, dose pathways and receptor ranking, inclusion onother Federal agency lists, and public or regional concern. Once theradionuclides of interest were selected, methods were chosen by theradiochemical method workgroup by applying the selection processdescribed above to the nuances of radiochemical analysis with particu-lar focus on: availability of published methods, the level of rigor withwhich the available methods have been validated, and the level of diffi-culty involved in implementing the method.

3. Developing analytical methodologies

3.1. Adaptation of methods to ensure fitness-for-purpose

Adaptation of some existing methods is technically possible for allcontaminant types. This adaptation may be possible when examplesare found in the literature which, based on scientific principles and con-sideration of contaminant characteristics, show promise for the neededcontaminant and sample combination. USEPA is adapting methods forcertain contaminant/sample combinations, and the resulting methodswill be considered for inclusion in later versions of SAM. Some of themethod development and adaptation activities that USEPA has per-formed in support of SAM are summarized elsewhere (USEPA, 2013d)or on the websites of their developers (USEPA, 2013a). A few examplesare provided below to show the range of activity.

One example ofmethod adaptation is for analysis of chemicalwarfareagents (CWAs) in environmental matrices. These CWAs belong to theclass of organic contaminants which are considered “semi-volatiles,”and existing USEPA methods were adapted to address the unique chal-lenges and characteristics of these CWAs, which are listed in Schedule 1of the Chemical Weapons Convention (CWC, 2004). Other examplesinclude development of sampling and analysismethods for chemicalwar-fare agent degradation products on environmentally relevant surfaces(Willison, 2012) and sewage sludge (Schuldt et al., 2013).

Further, USEPAMethods 538 and 540 were developed by USEPA fordrinkingwater analysis in support of various drinkingwater regulations(USEPA, 2013a). Some SAM contaminants not regulated in drinking

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Sample

BSL-2 or BSL-3 Bioagent

(Aerosol, Wipe, Swab, Drinking Water, Post-Decontamination Waste Water)

Sample Processing *

Drinking Water/ Post-Decon Waste Water

Concentration(As necessary)

Aerosol, Wipe, Swab

Culture Followed by Rapid Confirmation

(Real-time PCR, ELISA, other immunoassay)

ORRV-PCR (if available)

Rapid Analytical Method[(Real-time PCR, ELISA, other immunoassay)

OR (Culture-PCR/Immunoassay or RV-PCR)]

Post-DecontaminationCharacterization

* Neutralization of decontamination agents may be required for post decontamination phase samples.

Fig. 1. Flow diagram for biological sample processing based on real-world incidents. Methods in SAM are selected to be compatible with this process flow.

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water were included during the development of Methods 538 and 540.Also, methodologies for botulinum neurotoxin were adapted from acommercial immunoassay utilized for clinical and food samples andalso from an enzyme activity approach utilizingmass spectrometric de-tection (Raphael et al., 2012).

Biological methods include those for Escherichia coli O157:H7,Salmonella typhi, non-typhoidal Salmonella, and Vibrio cholerae O1 andO139 in drinking water, as well as Bacillus anthracis in soil. Thesemethods adapted existing analytical approaches to theparticular bacterialserotype and sample type of interest (USEPA, 2012b). USEPA has alsopublished a first-ever, web-based comprehensive protocol for detectionof B. anthracis from environmental samples (USEPA/CDC, 2012). This pro-tocol includes response-phase-appropriate, detailed, and step-by-stepmethods for sample processing and analysis for a variety of sampletypes, including water.

Fig. 2.Method development process for chemicals, biologicals, and biotoxins. The terminologytypes of samples may be applicable. Adapted from Shoemaker and Boutin (2008).

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3.2. Innovative methods developed to achieve SAM goals

In some cases, methods must be developed for certain contaminant/sample type combinations in SAM (Table 1). Fig. 2 illustrates the overallprocess in the development of chemical, biological, andbiotoxin analysismethods. The method development process for these contaminants in-cludes all steps between sample collection and data reporting, becauseof the interdependencies of technical requirements among steps. Forradiochemical contaminants, technical aspects such as sampling andholding time depicted in Fig. 2 do not have the same relevancy as forother types of contaminants (e.g., radioactive decay occurs at a known,unalterable rate). Due to the nature of radiochemical analysis, samplecollection for radiological contamination is separated from analysis,and information about radiological sample collection and the develop-ment of radiological sample collection plans for use during site

in this flowchart is based on instrument analysis of chemicals; other terminology for other

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characterization, remediation, and clearance phases appears elsewhere(USEPA, 2010c). Considerations for the development of radiochemicalmethods are discussed below.

The process depicted in Fig. 2 can be regarded as a fairly conservativedescription ofmethod development for chemical, biological, and biotox-in contaminants. Understanding the holding time of the method, andwhere possible selecting appropriate preservatives to maximize theholding time, is important for SAM methods, due to the potentialback-log of samples resulting from the sheer number of samples thatmay likely be collected from a catastrophic contamination incident(Magnuson et al., 2014). Another key aspect of the developed methodis its ability to meet the applicable DQOs. As these DQOs will be site-specific, it is necessary for themethod to perform as optimally as possiblein anticipation that state-of-the-science analysis of contaminant/sampletype combinations is required.

Applying Fig. 2 to achieve SAM goals, such as high throughput sampleanalysis and the ability for multiple labs to utilize themethod, has result-ed in the application and development of several innovative approaches.Some of these are innovative in that they apply technology and tech-niques not usually used for analysis of environmental samples. In otherexamples, the actual methodology and approaches are innovativein that they have not been extensively used for analysis in general,but provide an appropriate solution to the challenges of environmentalsample analysis in the circumstances for which SAM is designed to beused.

One example of techniques not usually used for analysis of environ-mental samples is the analysis methods for chemical warfare agentdegradation products on environmentally relevant surfaces (Willison,2012). Specifically, ultra-performance liquid chromatography (UPLC)was demonstrated to increase sample throughput over high perfor-mance liquid chromatography (HPLC), as illustrated in Fig. 3. WhileUPLC has gained ground for analysis in some fields, such as the pharma-ceutical industry, its adoption for environmental analysis has beenslower, perhaps because while permissible in some methods for envi-ronmental compliance, additional studies are required to ensure equiv-alence of the UPLC method to the HPLC method. Again, SAM methodsare not designed for environmental compliance, but examples such asFig. 3 demonstrate the throughput for various sorts of environmentalanalysis, including those for SAM purposes.

A specific example of innovation is the adaptation of analyticaltechnologies usually applied for clinical samples (e.g., blood and urine)for use with environmental samples. For instance, VX, an organophos-phate CWA, was analyzed in water and soil by immunomagnetic

Fig. 3. UPLC and HPLC retention time comparison of an approximate 50

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scavenging, a novel technique illustrated in Fig. 4 (Knaack et al., 2012;Knaack, Zhou and Magnuson 2013). This innovative sample preparationand analysis approach can be highly automated, with an estimated 800samples/day analyzed, with quantitation reporting limits in the low-parts-per-trillion range, making this analytical approach compatible forrisk-based toxicity criteria for VX (NRT, 2011).

Other high-throughput analysis methodologies also take advantageof robotic technology not usually utilized in environmental laboratories.Analysis of α-amanitin and biomarkers for ricin and abrin in drinkingwater was based on solid phase extraction followed by liquid chroma-tography tandem mass spectrometry detection (Knaack et al., 2013).Analysis of the rodenticide tetramine in water samples was achievedby automated solid phase extraction with gas chromatography/massspectrometry detection (Knaack et al., in press). These examples useequipment available in some public health laboratories, but themethodsutilized modify certain steps to allow appropriate method performancein environmental samples. The end result is a high-throughput methodwith characterized performance data for the environmental sampletype of interest.

Biological method development has focused on sample analysisthroughput and adaptation ofmethods and technology to environmentalsample types of interest. These include the use of commercial cleaningrobots for the sampling of Bacillus spores (Lee et al., 2013) and rapidviability polymerase chain reaction (RV-PCR) based detection ofB. anthracis (Letant et al., 2011; Shah, 2013) which combines thespeed and confirmation ability of PCRmethodswith the capability of cul-ture methods for determining viability. The overall process flow (Fig. 5)results in higher sensitivity, higher throughput, reduced interferencefrom environmental background, and possible faster turn-around, allwhile generating less waste.

An additional innovation was developed which fulfills the need inFig. 1 for “sample concentration (as necessary)”. Because relativelylow levels of biothreat agents can cause human health effects, sensitivedetection of these agents in drinking water is needed. Most rapidresponse analytical techniques assay small sample volumes or requirehigh concentrations of contaminants; therefore, large volumes ofwater should be collected and concentrated to enable sensitive detectionof biothreat agents. For this reason, USEPA (USEPA, 2011) developed afield portable (around 80 cm long × 50 cmdeep × 40 cm), automated ul-trafiltration device.

The development or adaptation of analytical methods for radiologicalcontaminants presents technical challenges that are sufficiently differentfrom chemical, biological, and biotoxin methodologies to warrant

0 ng mL−1 solution of four nitrogen mustard degradation products.

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Fig. 4. Immunomagnetic scavenging method for extracting VX from aqueous matrices.Magnetic beads conjugated to antibodies and BuChE are incubated in an aqueous matrixcontaining VX. The agent forms adducts with BuChE that are then digested into peptidesand analyzed by HPLC/MS/MS. Adapted from Sporty et al. (2010).

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separate discussion. Radiochemical methods are developed by USEPA forselect radionuclides to address challenges such as limited method avail-ability, difficulty of field detection with hand-held instruments, lack ofspecificity or verification for the isotope/matrix pair of interest, and lackof laboratory personnel with the knowledge and expertise to performthe method. The USEPA develops methods to address these issues. Themethods are designed to: a) withstand significant variations in chemicaland radionuclide interferences (i.e., robustness); b) address concernsabout handling and processing of potentially elevated activity materials;c) provide analytical turn-around times in the range of hours to days in-stead of days to weeks; and d) meet measurement quality objectives(MQOs) using the approach outlined in the Multi-Agency RadiologicalLaboratory Analytical Protocols (MARLAP) manual.

Newmethods developed by USEPA focus on expediting the analysisof sampleswhile providing quantitative results thatmeetmeasurementquality objectives applicable to the intermediate and recovery phases of anuclear or radiological incident of national significance. These methodsare designed to reliably achieve a pre-determined method uncertaintyof 13% at a radioactivity action level specified for the applicable (interme-diate or recovery) phase of the event. This establishedmethod uncertain-ty is intended to support appropriate decision-making for that phase ofthe event. SAM includes a number of these newly-developed, rapidmethods of radiochemical analysis in a variety of environmentalmatrices.

Fig. 5. Sample flow and timing in rapid viability polymerase chain (RV-PC

Please cite this article as: MagnusonM, et al, Analysis of environmental conoratory capability by selecting..., Environ Int (2014), http://dx.doi.org/10.1

These methods cut analysis time by 40–50% depending on the radionu-clide/matrix combination. Some of these rapidmethods are largely adap-tations of existing methods, employing innovative techniques to shortentime consuming steps while maintaining data quality. Other studies havedeveloped sample preparationmethods for certain types of environmen-tal samples, e.g., buildingmaterials, to enable the analysis of radionuclidesin these materials (USEPA, 2009).

4. Conclusion and future directions

The future of building and ensuring analytical capability and capacityfor environmental samples generated from catastrophic contaminationincidents may proceed along the same lines as in the past: adaptingand developing scientifically soundmethods to address the unique chal-lenges presented by environmental contamination resulting from cata-strophic incidents. For example, sample processing is still a bottleneckfor high throughput analysis, especially for certain sample types and dif-ferent types of agents (especially for the biological agents). No significantinvestment has been made to address this need for automated and highthroughput sample processing systems and methods for some contami-nants. One approach could be to develop stand-alone sample processingsystems for the most popular sample types and, where possible, inte-grated sample processing and analysis systems.

To increase the long-term sustainability of analytics designed for un-common occurrences, it may be useful to design these efforts to haveadditional benefit to other types of environmental analysis. For instance,the high throughput sample processing and analysis methods identifiedas a need for catastrophic events, may also help lower the labor and op-erating costs for analysis of samples taken for compliancewith environ-mental regulations. Similarly, by enabling a lower cost per sample, thenumber of samples used for environmental research studies could beincreased, leading perhaps to more comprehensive scientific conclu-sions and decisions. A final example of how additional benefits couldbe realized is by applying the analytical capability and capacity to bio-surveillance. Biosurveillance can be viewed as the first line of defenseagainst a number of types of catastrophes, and is increasingly thesubject of governmental initiatives and strategies (NSTC, 2013; USG,2012). Biosurveillance is the process of active data-gathering with ap-propriate analysis and interpretation of biosphere data thatmight relateto disease activity and threats to human or animal health –whether in-fectious, toxic, metabolic, or otherwise, and regardless of intentional ornatural origin – in order to achieve earlywarning of health threats, early

R) reaction approach compared with the traditional culture method.

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8 M. Magnuson et al. / Environment International xxx (2014) xxx–xxx

detection of health events, and overall situational awareness of diseaseactivity.

An important aspect of the future of contaminant analysis will beapplying the methods and approaches described above to all types ofcatastrophes, sometimes referred to as “all-hazards”. When doing this,it is important to note that the nature of the contamination releasescenario may affect the performance requirements of the analyticalmethod(s). Many of the activities described above have been relatedto the assumption that the contaminantwill be released as part of an in-tentional activity such as terrorism or criminal activity, resulting inwidespread contamination at low concentrations. However, considerthe example of natural disaster resulting in destruction of a chemicalstorage facility, leading to localized contamination present at a compar-atively high concentration. Because the SAM chemical methods weredesigned for lower concentrations, they might not perform well athigher contaminant concentrations unless changes are made to thesample preparation or instrumental analysis procedure. Adapting SAMmethods so that their performance requirements are tailored to addressanalytical needs in other catastrophe types is one future activity withsignificant benefits and relatively low resource requirements.

Disclaimer

The U.S. Environmental Protection Agency (USEPA), through itsOffice of Research and Development, performed, managed, funded,and/or collaborated in the research described herein. This content hasbeen peer and administratively reviewed and has been approved forpublication. Note that approval does not signify that the contents neces-sarily reflect the views of the USEPA. Reference herein to any specificcommercial product, process, or service by trade name, trademark,manufacturer, or otherwise does not necessarily constitute or implyits endorsement, recommendation, or favoring by theUnited States gov-ernment. The views and opinions expressed herein do not necessarilystate or reflect those of the United States government and shall not beused for advertising or product endorsement purposes.

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