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Environmental SRM Development J
ust three years after it was creAs EPA certification ated, the term "EPA-certified" is going the way of the dinosaur, acof environmental cording to officials in and outside the Environmental Protection Agency. After two reference standards is internal audits by EPA's Office of the Inspector General (OIG) and a lawsuit phased out, what—or brought by a chemical reference standards manufacturer, the EPA Environmental who—will replace Monitoring Systems Laboratory in Cincinnati (EMSL-Cin) agreed not to renew five this program is cooperative research and development agreements (CRADAs) it had awarded to unclear companies in 1991 to market environmen-
tal standards from the Repository for Toxic and Hazardous Materials and the Pesticides Repository. Under the CRADAs, which have been the focus of much controversy and some allegations of improper conduct at EMSLCin, EMSL-Cin distributed thousands of ampules to the companies in return for royalties on the sales. Three of those agreements have already expired; another one will expire by the end of the year, and the last one will lapse by January 1996. EMSL-Cin has made arrangements with the five companies to repossess and dispose of most of the unsold ampules it had given them to sell. The EPA-certified label created through these CRADAs will also be dropped after a grace period that depends on the stability testing schedule for each "neat" (pure form) or "synthetic" (mixture or solution) reference standard. Hanging in the balance are the definition and availability of EPA-certified reference standards. The discontinuation of this program also raises questions for analytical chemists about whether their results are valid and legally defensible. Al868 A
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though the language in most EPA methods allows most laboratories to use noncertified standards of equivalent quality, several branches of the federal government had recommended (and the State of Illinois and the government of Taiwan both had required) that their laboratories use only the EPA-certified standards. Reportedly, these groups are now backing away from the requirements in response to the phaseout. However, the OIG has found that some of the standards sold as EPA-certified weren't adequately tested for purity, identity, or stability. Moreover, some of the standards that tested poorly were nonetheless approved and distributed for sale. These findings may cast uncertainty over the validity of relying solely on EPA-certified standards for calibration and quality control. Also at stake is the security of some kind of regulatory oversight to ensure the quality and reliability of environmental standards on the market. What—or who— will replace the CRADA program set up by EMSL-Cin is not yet clear to the federal agencies, manufacturers, or third-party certifying organizations involved, although several proposals are being prepared. Creating EPA-certified standards
In the early 1970s, when EPA began to establish regulations that mandated environmental testing for hazardous chemicals, few reference materials for quality assurance (QA) existed. Through its QA program, EMSL-Cin started making and distributing reference standards to qualified users free of charge. Over the years, as the number of different regulated analytes multiplied and tolerance levels for
An Ampule of Controversy
some chemicals dropped, EMSL-Cin farmed out the development and manufacture of new standards to contractors. By 1990 its inventory had swelled to about 750,000 ampules with a potential market value of $26 million, according to OIG estimates. But the laboratory was incurring greater and greater expenses to run the expanded program. In 1986, the Office of Management and Budget allowed EPA to charge user fees for the standards, but the money had to be deposited in the U.S. Treasury and would not necessarily be returned to the QA program. At the same time, funding for the free standards distribution program was permanently eliminated in anticipation of a user-fee setup that was never implemented, and EMSL-Cin was forced to look for other sources of support. However,
that year Congress also passed the Federal Technology Transfer Act (FTTA), which allowed federal agencies to establish CRADAs with the private sector for R&D. Certain types of revenue that came into a federal agency or branch from one of its CRADAs could be kept and used to fund its programs. In 1989 and 1990, EMSL-Cin asked standards manufacturers for CRADA proposals to privatize the maintenance and distribution of its existing standards and provide for R&D and manufacture of new stocks. In 1991, it negotiated the five CRADAs with Ultra Scientific; Spex; Supelco; Fisher Scientific, which later sold out to Resource Technology; and NSI Environmental Solutions, a subsidiary of longtime EPA contractor Man-Tech. For the first time in almost 20 years, EPA stan-
dards would be sold by the 5 companies at market prices father than provided free. The limited number of CRADAs issued and the market advantages conferred by them incensed a number of the CRADA companies' competitors. One of those who filed complaints with the OIG was Mark Carter of Environmental Resource Associates (Arvada, CO). He requested EPA documentation through the Freedom of Information Act for the CRADAs, the repository inventory, and purity and stability testing data for the repository standards and newly manufactured CRADA materials. On the basis of these documents, he protested the validity of the term EPA-certified, the legality of the CRADAs, and the assumed quality of the standards. The complaints he and others filed led to two internal OIG audits of the EMSL-Cin QA materials program, one to examine the propriety of the CRADAs and assess their effect on the marketplace, and the other to investigate allegations that the standards being marketed were not properly tested and were not all of the quality stated on the label. The hand that rocks the CRADA
The CRADAs were unusual in several respects. In its audit report of March 31, 1993, the OIG noted that the agreements were competed "much like contracts," that no new technology appeared to be transferred, that the CRADAs not only allowed but required use of the term EPA-certified and allowed exclusive use of the EPA logo, that the agreements contained no accurate account of the value and quantity of inventory transferred to the companies, and that among thefivehighly similar CRADAs the differences in royalty per-
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centages varied from 8% to 50% for sales of existing EPA inventory and from 5% to 25% for newly manufactured materials. Although the OIG declined to say that the CRADAs appeared illegal under the FTTA, it concluded in its first report that they were an "inappropriate use" of the FTTA; did not transfer new technology; appeared to pose a conflict of interest, particularly with regard to one of the CRADA companies; created conditions for a potential government-controlled monopoly; and did not adequately control the companies' handling of transferred and marketed reference standards. As evidence of a skewed market with the potential for a monopoly, the OIG cited a sharp increase—an average of fivefold—in the price of several standards between 1990 and when the CRADAs were established. The price of one pesticide neat, strobane, jumped from $0.04/mg to $6/mg in less than a year. "We were unable to obtain a reasonable explanation," the OIG reported. "In most discussions there was some denial of any increase or very general comments regarding cost increases to cover increased expenses. .. each company received a substantial inventory for free, and these companies were already in the business. If anything, the prices should have been lower." The OIG said that EPA should not put itself in the position of competing with private industry and recommended immediate cancellation of the CRADAs.
regarding the amount of testing conducted, the adequacy of certification protocols, the extent of EPA reviews, and the determination of stability testing schedules." In several cases, the stability testing, which went on a doubling schedule (0 days, 30 days, 60 days, etc., up to 4 years), was simply not done for some of the repository stock. The stability testing schedules for each type of reference standard are what EMSL-Cin has proposed to use as the guide for determining when that standard's EPA-certified status will be cancelled. Instead of cancelling the CRADAs outright, EMSL-Cin stated that it preferred to let them lapse, recall the EPA repository materials, disallow use of the EPA logo by the CRADA companies, and allow a grace
ing the CRADA companies' customers that some of the EPA-certified repository reference materials sold to them after 1991 may not be reliable either. EMSL-Cin did arrange to have all other repository materials either reformulated and certified to CRADA specifications or recovered by EPA earlier this year. Policy versus legality
These audits provided no legal direction on the establishment of the CRADAs, according to EPA Patent Counsel Thomas Gorman. "There are two issues here, policy and legality," he says. "People tend to get them confused." In February 1992, however, Chem Service (West Chester, PA), which manufactures and sells environmental reference standards, sued EMSL-Cin for awarding three of the five CRADAs to the company's competitors. It alleged that the CRADAs were in fact government procurement contracts and not R&D agreements. It also alleged that the standards being sold as EPA-certified did not meet and were not held to the criteria that had been established for them under the CRADAs and then shared with the American Association for Laboratory Accreditation (A2LA) in 1991 through a Memorandum of Understanding (MOU). Chem Service argued that third-party certification by A2LA was rigorous and expensive, but it was the only way for nonCRADA companies to be sure EPA would accept their products for mandated testing period for terminating the use of the words methods. "EPA-certified" on their products. Under A district court accepted EPA's motion Unstable testing data this scheme, most of the companies' stan- to dismiss and ruled that Chem Service dards would cease being marketed as was not in the "zone of interest" (type of In December 1992 the OIG began a second internal audit of EMSL-Cin to find out EPA-certified by 1997; NSI Environmental company or party) that Congress had inSolutions would be allowed to keep some tended to protect with the FTTA and therewhether the inventory of reference standards transferred to CRADA companies of the repository stock (initially, 4% of al- fore had no standing to sue the EPA. most 500,000 ampules distributed to it; However, the appeals court overturned had been tested to CRADA specificathat decision and reinstated the suit on tions before being sold as EPA-certified. In after July, only 2.5%) until the end of this Dec. 27,1993. a Feb. 7,1994, report the OIG stated, "We year. Some of its own manufactured standards could be called EPA-certified until as found several instances where selected That court's ruling expanded the interpre-CRADA QA materials identified in the late as 1999 (see Table 1). EMSL-Cin's di- pretation of zone of interest to include the rector, Thomas Clark, also sent out a letallegation lacked manufacturing criteria Federal Procurement Act which, accordand supporting data, did not meet proto- ter to purchasers notifying them that stan- ing to Chem Service, EMSL-Cin had viodards obtained from the EPA repositocol requirements, and were approved by lated with the CRADAs. If the CRADAs ries before 1991 are no longer reliable. EPA despite poor test results. The data were in fact used to circumvent the open These measures have been accepted by supporting the quality of materials probidding process required by that act, as the OIG, which has closed its audits of duced under the CRADAs [newly manucontended, then Chem Service did have EMSL-Cin. factured standards] was more organized standing to sue, the appeals court ruled; and complete However, for [these] mabut it noted that A2LA certification was However, neither the OIG nor EMSLterials, we identified some weaknesses not mandatory for the company and that Cin has addressed the problem of notify870 A
Under this scheme, most of the standards would no longer be marketed as EPA-certified after 1996.
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the FTTA did not give it standing to sue the EPA over the MOU. (A dissenting judge in the appeals court thought Chem Service had standing for this second charge as well.) The suit was being pur sued at press time Quly 1994) but, accord ing to Lyle Phifer, a part owner as well as vice president and technical director of Chem Service, a court date—with the judge who originally dismissed the case— had not yet been assigned. If Chem Service wins, says Phifer, the CRADAs may be cancelled immediately by court order rather than being allowed to lapse, and so may the existence of the term EPA-certified. However, EPA has not cancelled the MOU for EPA-acceptable third-party certification of environmental standards, and A2LA is continuing to par ticipate in the program—although it's un clear whether the MOU still has mean ing or, if it does, what that meaning is.
zations such as A2LA, and a consortium of to QA. Some of the problems with defin ing traceability of secondary reference ma chemical reference materials manufac terials to the national standards, Reed says, turers. are integral to the chemistry involved. Defining traceability The ISO guidelines define traceability McKee says that EPA and NIST are work in terms of an "unbroken chain of compar ing out an agreement whereby NIST ison" between a nationally recognized would coordinate a third-party certifica standard and a commercially produced tion process. "I think it's NIST's desire as material. "For physical measurements," well as my own to involve the manufactur says Reed, "traceability is pretty well ers in this process," he explains. At this understood. But in chemical measure year's Pittcon, NIST and the American ments, sampling, separations, and the Chemical Society (ACS) held a joint work matrix itself can cause problems." Finding shop on defining and creating traceabil ways to define the unbroken chain of ity links between nationally accepted envi comparison between neat standards and ronmental standard reference materials those found in natural matrices such as (SRMs) and those produced commercially soils or vegetation is one of NIST's ob in bulk. jectives. Chem Service's Phifer adds that for William Reed, former chief of the SRM program at NIST, says, "In the past, NIST many environmental reference materials, purity is not assayed directly. He says, has supplied SRMs for environmental work in limited quantity and only provided "There are several different methods of approach for purity analysis, and there a small part of the variety needed. Now aren't a lot of references in the literature Into the breach NIST has made a change in its approach. We're trying to figure out ways to boost on this." For pure materials (95-100%), According to Gary McKee, deputy direc the most precise methods are subtractive tor of EMSL-Cin, EPA is preparing to step the linkage between our materials and rather than direct because the relative the commercial ones to make secondary back from its traditional oversight role precision of instrumental determinations reference materials credible and legally for the production of reference standards is usually 1-2%. The contaminants in the and is not likely to reinstate the EPA certi defensible." sample are determined and subtracted fication process it has followed in the past One possibility discussed at the work three years. "EPA certification is going to shop was the adoption of the International from 100%, but, Phifer says, "You don't know specifically what contaminants are be nonexistent," he says. "One thing Organization for Standardization (ISO) present. We use multiple subtractive that's obvious is that we are moving out of definitions for traceability and stability methods and try to make sure the re the CRADA process for QA materials." testing, which stem from a scientific, sults agree." rather than legal or regulatory, approach Instead, he says, EPA will concen trate on developing protocols for ensuring the quality and availability of marketproduced reference materials required for Table 1 . Status of EPA-certified pre-CRADA repository stock a n d n e w materials 1 regulatory testing. "It's apparent to me Expiration of Company Pre-CRADA Return of preLast CRADA 3 that we're not going to use the same mech EPA certification stock received CRADA stock stability tests | anism for all groups of materials. For in to EPA for new stock | on new stock stance, metals standards and materials are Supelco ~105,000 ampules complete 1/31/94 1991-1993 early 1995 < generally of high quality and widely avail ο (44 materials) X able; for pesticides, this is less true. We ο want to target our involvement to areas Ultra Scientific -440 pesticide 370 after 12/31/93 1991-1992 1995-1996 jjj where the marketplace isn't meeting the neat materials 70 blended and ô retained need." To help determine the state of the marketplace, McKee says, EPA has sent 1991-1992 1995-1996 ν Spex Industries ΙΝΑ complete 1/3/94 en σ> out a survey to regulatory labs and is con ducting an in-house study of the availabil 1991-1992 1995-1996 | Resource 19 QA materials in 16 by 1/31/94 Technology various quantities ~25% of 3 blended ity of reference standards. < materials retained Who willfillthe QA gap for the market Ο sectors EPA decides not to focus on, and 1996-1997 s NSI -500,000 ampules 96% by 1/1/94 1992-1993 1999 t Environmental 97.6% by 7/1/94 4-year test for how will they do it? The choices include Solutions complete 1/1/95 1991 materials other federal agencies such as the Na in 1995 tional Institute of Standards and Technol ΙΝΑ- information not available
