Environmental As EPA certif;ication of environmental reference standardk is phased out, w h a t - o r who-will replace this program is unclear
ust three years after it was created, the term “EPAcertified” is going the way of the dinosaur, according to officials in and outside the Environmental Protection Agency. After two internal audits by EPA’s Office of the Inspector General (OIG) and a lawsuit brought by a chemical reference standards manufacturer, the EPA Environmental Monitoring Systems Laboratory in Cincinnati (EMSLCin) agreed not to renew five cooperative research and development agreements (CRADAs) it had awarded to companies in 1991 to market environmental 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 EMSL Cin, EMSLCin 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. EMSLCin 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 availabilityof EPAcertified reference standards. The discontinuation of this program also raises questions for analytical chemists about whether their results are valid and legally defensible. Al-
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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 EPAcertified weren’t adequately tested for purity, identity, or stability. Moreover, some of the standards that tested poorly were nonetheless approved and distrib uted for sale. These findings may cast uncertainty over the validity of relying solely on EPAcertified 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-r whowill replace the CRADA program set up by EMSLCin is not yet clear to the federal agencies, manufacturers, or third-party cert3jing organizations involved, although severalproposals are being prepared. Creating EPA-certified standards In the early 1970s, when EPA began to es-
tablish regulations that mandated environmental testing for hazardous chemicals, few reference materials for quality assurance (QA) existed. Through its QA program, EMSLCin 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 Ampde 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 EMSLCin was forced to look for other sources of support. However,
that year Congress also passed the Federal Technology Transfer Act (%?TA), 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, EMSLCin 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 fi-ee. 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 EMSLCin 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 the five highly 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 FITA, it concluded in its first report that they were an “inappropriate use” of the FIT& 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 $O.O4/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. Unstable testing data
In December 1992 the OIG began a second internal audit of EMSLCin to find out whether the inventory of reference standards transferred to CRADA companies had been tested to CRADA specifications before being sold as EPA-certified. In a Feb. 7,1994, report the OIG stated, ‘We found several instances where selected preCRADA QA materials identified in the allegation lacked manufacturing criteria and supporting data, did not meet protocol requirements, and were approved by EPA despite poor test results. The data supporting the quality of materials produced under the CRADAs [newly manufactured standards] was more organized and complete. .. . However, for [these] materials, we identified some weaknesses
regarding the amount of testing conducted, the adequacy of certificationprotocols, 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 EMSLCin 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, EMSLCin 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. EMSLCin did arrange to have all other repository materials either reformulated and certified to CRADA specificationsor 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 EMSLCin 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 LaboratoryAccreditation (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. A district court accepted EPA’s motion “EPA-certified”on their products. Under this scheme, most of the companies’ stan- to dismiss and ruled that Chem Service was not in the “zone of interest’’ (type of dards would cease being marketed as EPA-certified by 1997; NSI Environmental company or party) that Congress had intended to protect with the FITA and there Solutions would be allowed to keep some of the repository stock (initially, 4%of al- fore had no standing to sue the EPA. However, the appeals court overturned most 500,000 ampules distributed to it; that decision and reinstated the suit on after July, only 2.5%)until the end of this Dec. 27,1993. year. Some of its own manufactured stanThat court’s ruling expanded the interdards could be called EPA-certified until as late as 1999 (see Table 1). EMSLCin’s di- pretation of zone of interest to include the Federal Procurement Act which, accordrector, Thomas Clark, also sent out a letter to purchasers notifying them that stan- ing to Chem Service, EMSLCin had violated with the CRADAs. If the CRADAs d.ards obtained from the EPA repositowere in fact used to circumvent the open ries before 1991 are no longer reliable. bidding process required by that act, as These measures have been accepted by contended, then Chem Service did have the OIG, which has closed its audits of standing to sue, the appeals court ruled; EMSL-Cin. but it noted that A2LA certification was However, neither the OIG nor EMSL not mandatory for the company and that Cin has addressed the problem of notify-
Under this scheme, most of the standards would no longer be marketed as EPA-certified afler 1996.
870 A Analytical Chemistry, Vol. 66, No. 17, September 1, 1994
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 pursued at press time uuly 1994) but, according 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 casehad 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 EPAcertified. However, EPA has not cancelled the MOU for EPA-acceptable third-party certification of environmental standards, and A2LA is continuing to participate in the program-although it’s unclear whether the MOU still has meaning or, if it does, what that meaning is.
Into the breach According to Gary McKee, deputy director of EMSL-Cin, EPA is preparing to step back from its traditional oversight role for the production of reference standards and is not likely to reinstate the EPA certification process it has followed in the past three years. “EPA certification is going to be nonexistent,” h e says. “One thing that’s obvious is that we are moving out of the CRADA process for QA materials.” Instead, he says, EPA will concentrate on developing protocols for ensuring the quality and availability of marketproduced reference materials required for regulatory testing. “It’s apparent to me that we’re not going to use the same mechanism for all groups of materials. For instance, metals standards and materials are generally of high quality and widely available; for pesticides, this is less true. We want to target our involvement to areas where the marketplace isn’t meeting the need.” To help determine the state of the marketplace, McKee says, EPA has sent out a survey to regulatory labs and is conducting an in-house study of the availability of reference standards. Who will fill the QA gap for the market sectors EPA decides not to focus on, and how will they do it? The choices include other federal agencies such as the National Institute of Standards and Technology (NIST), third-party certifying organi-
to QA. Some of the problems with defining traceabilityof secondary reference materials to the national standards, Reed says, are integral to the chemistry involved. The IS0 guidelines define traceability Defining traceability McKee says that EPA and NIST are work- in terms of an “unbroken chain of comparison” between a nationally recognized ing out an agreement whereby NIST standard and a commercially produced would coordinate a third-party certificamaterial. “For physical measurements,” tion process. “I think it’s N I T S desire as well as my own to involve the manufactur- says Reed, “traceability is pretty well understood. But in chemical measureers in this process,’’ he explains. At this ments, sampling, separations, and the year’s Pittcon, NIST and the American Chemical Society (ACS) held a joint work- matrix itself can cause problems.” Finding ways to define the unbroken chain of shop on defining and creating traceability 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 objectives. in bulk. 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 NIST has made a change in its approach. aren’t a lot of references in the literature We’re trying to figure out ways to boost on this.” For pure materials (95-loo%), the most precise methods are subtractive the linkage between our materials and rather than direct because the relative the commercial ones to make secondary reference materials credible and legally precision of instrumental determinations defensible.” is usually 1-2%. The contaminants in the sample are determined and subtracted One possibility discussed at the workshop was the adoption of the International from loo%,but, Phifer says, “You don’t know specificallywhat contaminants are Organization for Standardization (ISO) present. We use multiple subtractive definitions for traceability and stability methods and try to make sure the retesting, which stem from a scientific, rather than legal or regulatory, approach sults agree.” zations such as A2LA, and a consortium of chemical reference materials manufacturers.
Company
Pre-CRADA stock received
Return of preCRADA stock to EPA
Supelco
-105,000 ampules complete 1/31/94 (44 materials)
Last CRADA stability tests on new stock
Expiration of EPA certificatioi for new stock
1991-1993
early 1995
1992-1 993 4-year test for 1991 materials in 1995
1996-1 997 1999
Spex Industries INA
NSI -500,000 ampules 96% by 1/1/94 Environmental 97.6% by 7/1/94 Solutions complete 1/1/95 INA = information not available
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Direct methods such as gravimetryand titrimetry don’t always exist for organic materials. However, says Phifer, ‘We often use acid and base titrations as an additional check to detect whether major errors have occurred.”
don’t rely on just one product; they buy the same standard from several different companies and cross-test them, because the cost of the materials is less than their liability for doing something wrong.”
Traceability and certification
However, most observers in and outside the government agree that some quality specscations will have to be created so that everyone will know how to meet the criteria for mandated EPA methods. Two possible players are a newly formed chemical reference materials manufacturers association and the ACS Analytical Reagents Committee, which has been asked to write specifications for environmental standards along the lines of the ones for “ACS reagent grade” chemicals. The new association, which is being organized by a steering committee of reference materials manufacturers set up by Chem Service, will probably accept federal agencies as associate members and will address environmental and nonenvironmental uses for reference materials. The committee has obtained a nonprofit corporate charter, and its organization and activities were discussed at the EnvirACS meeting in July in Washington, DC. Approximately 20 manufacturers from the domestic industry took part in a spirited exchange and agreed to participate in ongoing discussions. Reed says he doesn’t mind that the participants at the Pittcon workshop rejected his suggestion of a NIST secretariat for the group. Reed, Phifer, Carter, and Keith all agree that the association could provide the industry with a unified voice for presenting its views and needs to agencies such as NIST and to federal and state regulatory organizations. According to committee secretary William Schmidt of George Washington University and committee chairman Paul Bouis of J. T. Baker, the ACS Analytical Reagents Committee has just begun to consider whether it should try to develop quality specifications for the neat chemicals used to make organic and inorganic environmental standards, which are often mixtures. If the committee decides to take on the project at its next meeting in October, ACS could embark on a new role in regulatory environmental testing. Deborah Noble
Unibing the language
In
