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Jeanette G. Grasselli Department of Chemistry Ohio University Athens, OH 45701
Our ability to determine the structure and composition of materials in all media has grown in amazingly exponential ways over the past several decades. Furthermore, there is no reason to believe that this pattern will slow down in the near future. The impact on the industrial sector of this increased capability to analyze products and understand mechanisms has been breathtaking. Advances in biotechnology, medicine, electronics, catalysis, chemicals, polymers, and new materials would not have been nearly so spectacular without the leverage available from new analytical techniques. Figure 1 illustrates t h e rapid changes in detection limits, sample size, and analysis time that have occurred in analytical science since World War I1 (1). Detection limits have gone from the microgram to the subpicogram level. A millimeter sized sample presented a challenge in 1950; today we routinely look a t submicrometer units or even at sinThis article is adapted from a presentation at the 13th Annual Meeting, Council for Chemical Research, Midland, MI, October 1991.
0003- 2700/92/0364-677A/$02.50/0 0 1992 American Chemical Society
of elements and molecules 1 quantities in increasingly complex matrices
gle atoms resolved in analytical electron microscopes. Analysis times have decreased from the hours or sometimes even days required for a complete qualitative and quantitative analysis. Modern capabilities, including real- time spectroscopy for in situ experiments, can provide data on molecular dynamics in the femtosecond time range. Marie Curie once said, “Nothing in life is to be feared; it is only to be understood.” Analytical science today is indeed the catalyst and key to our understanding. Trace analysis, the detection and determination of incredibly tiny
(such as environmental samples), is readily accomplished today. Yet some people tend to view analytical advances as a negative factor in environmental studies because the ability to measure extremely small quantities can focus regulatory restrictions on materials not previously detect able. This is a rare instance in which increased knowledge can be considered a setback. The ability to “see” previously invisible components has both good and bad sides. On the good side, we can identify components t h a t are truly deleterious; on the other side, we ean initiate witch hunts for no other reason than that a material can be detected or measured. Thus we must ask: Is analytical chemistry feeding the environmental revolution? Should we be concerned with improving our detection limits for preselected target analytes? (These are our current concerns, driven by environmental regulations that have also grown exponentially, as shown in Figure 2 [Z].) Or would it be 9 more value to industry and society to direct our analytical efforts toward identifying “all” the components in environmental samples, thereby providing early warning of impending environmental threats or hazards to human beings and biota? Analytical
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REPORT science could then feed the technological advances that would allow us to mitigate environmental changes or adapt to them. This brings to a focus the other side of the question, the issues of risk assessment, risk management, and risk communication. These terms, along with “detection limits,” “selectivity,” “accuracy,” “analytical vari ability,” “quality assurance,” and “total quality management,” must be defined and made understandable to the public, regulators, and the industrial establishment. We can no longer separate the performance of science from the mandate to communicate our findings and uncertainties to the public. What role do analytical chemists
play in industrial and environmental science, and how can they be deployed most effectively? How should they influence t h e quantity and quality of communication between their laboratories and legislative or public interest groups? I t is critical that we have a better understanding of the risks presented by environmental releases; they must be stated in terms that allow the public to gain a realistic measure of the effects of exposure. How easy it is to forget that life expectancies in the United States have risen nearly 50% in our lifetimes while the public has been bombarded by media reports of increasing threats from pollution. Admittedly, all is not well, but neither are we facing catastrophe. Most com-
Figure 1. Technical progress in detection limits, sample size, and analysis time.
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Figure 2. Legislative mandates from 1945 to 1995. 678 A
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panies have addressed environmen tal issues positively and forthrightly. However, if senior management does not set clear ethical standards for subordinates and enforce them, there is considerable opportunity to take environmental issues lightly, or in rare instances to ignore them. Role of the analytical chemist in environmental science In more than 30 years of industrial experience, I have been involved in research in chemical processing; catalysis; biotechnology; new materials; and, most of all, analytical and environmental science. I have been part of and have watched the “analytical revolution” and its impact on industrial, medical, and academic research, and I have developed strong feelings on the most effective use of analytical chemistry in addressing industrial and societal problems. With the exception of routine, repetitive analytical testing, i t is a mistake to consider measurement as the primary role of analytical chemists. They must be problem solvers. Too many laboratories consign their analysts to pigeonholes where they function as sample drop-off points. In this mode of operation we lose much of the power of both the analyst and the sample submitter. The analytical chemist should be an active participant i n problemsolving teams from the outset. Thus the analyst gains useful insight into the totality of the problem-including, for example, knowledge of feedstocks, processing conditions, recovery methods, and potentially related byproducts. In turn, with this knowledge the analyst can suggest Sampling methods and a combination of analytical techniques best designed to monitor any problems. It seems illogical that the analyst not be involved in establishing the best means for the collection of meaningful and representative samples and the ap propriate order of analysis. In addition, it is important that the analyst on a particular problemsolving team take a broad view of the techniques that might be used. In these days of complicated, hyphena t e d , multitechnique analytical methods, t h e power of combined techniques should be obvious. Finally, the function of the analytical chemist is to provide information of a sufficiently valid nature, that is, of the requisite statistical significance so that meaningful decisions can be made. Analytical scientists must take responsibility for the informa tion they provide.
I have found that the most import a n t contributions of a n a l y t i c a l chemists have come from the elucidation of mechanisms rather than from the simple determination of levels of concentration (e.g., understanding how a sample catalyst works or the sequence of addition of molecules in a polymer synthesis). In environmental areas, the potential major contribution of analysts could be in spelling out the toxicological mechanism by which a chemical affects human processes. Public policy and perception The Pimentel report “Opportunities in Chemistry” ( 3 ) proposed that the EPA follow exactly this model in four recommendations related to the environment. The first asked for a n increase in the percentage of EPA R&D funding devoted to exploratory research, particularly research on environmental problems of the future. The second encouraged systematic and fundamental research on clarifying reaction pathways for substances of environmental interest. The third called for efforts to detect potentially undesirable environmental constituents a t levels well below known or expected toxicity limits. But only when compounds are identified can their risks and benefits be assessed and decisions made regarding use and exposure (4). Finally, it was recommended that EPA support analyt ical chemistry research in a prominent way. The report called for increased ability by regulators to measure and detect contaminants. Such ability requires close collaboration between toxicologists and analytical chemists ( 5 ) . EPA Administrator William Reilly a n d h i s Science Advisory Board appear to be in consonance with these recommendations. A recent article (6)focused on attempts to “give science a bigger role in EPA policy” and described the problem of refocusing EPA research into more promising areas. It states that 80% of the agency’s budget is fixed for all practical purposes and that an additional 15%has been directly targeted by congressional action, leaving only about 5% truly flexible. Reilly asked for four-year plans focusing on risk reduction rather than on meeting the latest court-ordered deadline to determine t h e level of a toxic substance. The article concludes that not only must EPA change its approach, b u t Congress a n d t h e Office of Management and Budget must also adopt similar change8 in culture and base their direction on scientific,
rather than political, grounds. Such progress is not likely to be rapid. Should EPA in particular and industry in general follow this path of intensifying their analytical efforts and generating new results, the communication issue will come to the fore. The change over the past 10 years in the public’s perception of health risks posed by chemicals has been documented by Vincent Covello of Columbia University (7,8). Ten years ago most people in the United States believed that 10% of all cancers were caused by lifestyle factors such a s smoking, diet, and lack of exercise; that another 10% were caused by exposure to chemicals in the environment; and that the remaining 80% were attributable to fate or natural causes. Today, however, most people still believe that 10% of all cancers are caused by lifestyle factors, but they attribute 5% to fate and the remaining 85% to chemical exposure. An even more alarming finding is that most science teachers believe that 80% of all cancer cases result from chemical exposure. This research indicates that industry and government have lost substantial credibility, because the public perceives them as dishonest, incompetent, and uncommitted to solving environmental problems. This distrust makes a difficult communication even harder. Covello proposes three steps for bridging the credibility gap. First, government and industry must make a concerted effort to win back the public’s trust and credibility by showing that they are honest, competent, caring, and committed to solving environmental problems. Second, they must draw on the credibility of those whom the public still trusts, such as medical doctors and university scientists. Third, government officials need to improve their risk communication skills. As these improved skills are used, the public’s understanding of chemical safety and risk will i n crease. Behind this generic problem of distrust lie some true communication barriers. The most obvious is that our papers a r e filled with jargon (e.g., “ESCA and “CAT scan”) and jaw-breaking words (e.g., “picosecond,” “intercellular molecular activity,” and “postmitotic growth). These simply must be put into clear English without compromising the validity of the research. Almost as difficult is the task of explaining environmental risk in ways t h e public can understand.
Richard Wilson, a Harvard physicist, has attempted this (9) by expressing deaths per kilowatt hour caused by producing electricity by various means. His intent is to show that nuclear power produces fewer fatalities than most other schemes of producing electricity. This terminology is probably satisfactory for scientists, but the lay public may have trouble d i s t i n g u i s h i n g w h e t h e r lo-’ is greater or less than 10-l’. Wilson rejects the idea that perception of risk is more important than the magnitude of risk. The public is diverse and perceptions change-but t h e risk stays the same. Therefore it is even more important to understand and appreciate strengths and weaknesses in the a n alytical methodology used in environmental science, and to explain the uncertainties in toxicological data. Sampling errors often are very large at low concentrations in real-world samples (10, 11),and toxicological activity falls off rapidly (and not linearly) a t low levels (12).In addition, natural toxins in our diets greatly exceed synthetic ones (131, and because nothing is without risk, we must find better means of doing and expressing cost-benefit analyses (14).Finally, dosages in animal testing often cause cell damage before carcinogenic action begins and perhaps initiate it (13). State of the art in environmental analytical science As shown in Figure 1, the state of the a r t in analytical science for the type of trace analysis involved in environmental samples is impressive. But other issues must also be considered. These involve the state of the practice related to the state of the art, the uncertainty in sampling for trace analysis, and the relationship between what can be measured and what is harmful to human health. Most of us are rightly frightened of cancer. We can measure substances, such as those synthetic chemicals determined to be toxic (and therefore regulated by the Delaney Clause to zero level in or on food), to extremely low detection limits. Walter Harris of t h e University of Alberta h a s pointed out that, during the past two decades, t h e detection limit h a s dropped from a concentration near that which produces a measurable dysfunction in a human to a concentration that may be 6 or more orders of magnitude lower (see Harris’ related REPORT on p. 665 A). In short, there is no scientifically provable way to test the validity of the extrap-
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olation. I n addition, Hutchinson pointed out in 1964 that the probability of an element having a function decreases with decreasing concentra tion (15). New studies by Ames and Gold (13) argue with the animal tests that lead to estimates of whether substances cause cancer. They believe that early work was based on inaccurate ideas about how cancer comes about, and therefore unwarranted assumptions were made about the degree to which data gained from high doses of chemicals can reveal anything about the effects of low doses. Ames’ recent work also shows that there are naturally occurring pesticides present in concentrations a hundred or more times higher in fruits and produce than are any synthetic chemicals. With this perspective, and in the midst of the furor, analytical chem-
ists face their own dilemma with regard to the real-world sources of uncertainty and error in the data they obtain. Although sources of error such as sampling, contamination, and selectivity are recognized, they are extremely difficult to overcome in practice. As a result, at a concentration of 1 ppb, the average uncertainty found for a variety of methods carried out in different labs has been close to f 50%. Furthermore, the uncertainty rapidly grows larger as one goes to lower concentrations. The lack of quality control in environmental sample analysis has been discussed by Hertz (2), and an example is shown in Table I. In this study, conducted by the National Bureau of Standards (now the National Institute of Standards and Technology, or NIST), Hertz pointed out that the results obtained from various laborato-
Figure 3. Effect of spiked concentration on the percentage of laboratories reporting results within f 40% of true concentration of benzene. (Adapted with permission from Reference 15.)
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ries conducting routine tests on round-robin samples fell far short of the accuracy and precision achievable under the best of good laboratory practices by qualified chemists. For example, one of the supposed PCB samples had no Arochlor (PCBs) added, and NBS analyses confirmed that no PCBs were present at the limit of detection of the method. Yet nine of the 18 laboratories reported the presence of PCBs, and one laboratory reported a high value of 113 ppm. Factors contributing to the variability in results include samplehandling procedures, purity of reagents and sample contamination from other sources, conditions of facilities and equipment, and the lack of available reference or calibration materials for standardization. I n a n o t h e r s t u d y reported by Stanko and Hewitt of Shell Development Company (151, the performance of 20 contract laboratories using EPA Method 8020 for determination of purgeable organics in groundwater was evaluated. Ten groundwater samples were submitted blindly to the laboratories, all of which had been used for RCRA compliance monitoring by Shell. Nine of the samples were spiked with various concentrations (0.12- 18 pg/L) of benzene, toluene, and xylenes. The mean recovery for all compounds ranged from 43% to 150%. Most labs met the precision criteria, but at concentrations < 20 pg/L the overall precision estimated by the EPA method could not be achieved. There was much confusion among the labs on detection limits, and those reported by the laboratories indicated that they had overestimated their ability to actually quantify analytes of interest in real matrices. Figure 3 shows the results for the PQL (practical quantifiable limit) for benzene. The PQL is the concentration at which 80% of the labs recover 40% of the true amount of the analyte, and the PQL specified for these chemicals in groundwater (under 40 CFR Part 264, Appendix IX) is 2 pg/L. It is obvious from the results of the audit on the contract laboratories that the PQL for the method is actually -7.5 pg/L when real groundwater samples are used. Of even greater concern is the number of compounds that may not have been extracted by c u r r e n t methods, or that may have been extracted but not determined, and that might pose a serious threat to human health. It is estimated that 99% of the organic compounds in most environmental samples are ignored (5).
Richardson et al. (16) have addressed the impact of hyphenated techniques and multispectral analy sis on this issue. Figure 4 shows the multispectral identification of aldehydes in municipal effluent. Total ion current GUMS and GC/FT-IR spectroscopy were used along with low- and high-resolution electron impact and chemical ionization MS to identify eight straight -chain alde hydes in a water sample taken from the overflow pipe of a municipal sewer line that contained a combination of industrial and domestic sewage. The appearance of straightchain aldehydes was unexpected and considered significant. Such aldehydes could arise from bacterial metabolism or from ozonolysis of drinking water (a treatment currently being considered to replace chlorination in the United States and already widely used in Germany). Concern about the presence and identification of aldehydes stems from studies showing that they cause nerve damage in animals, especially those with diabetes. The exact identification of these compounds could not have been made without the use of the combined chromatographic and spectral techniques and t h e availability of spectral reference data banks. Thus the multispectral approach has great potential in the field of environmental analytical chemistry, and it is actively supported by the EPA labs (4,5, 17). Risk assessment In light of the tremendous current capabilities of analytical science and the inherent difficulties in realizing those capabilities in a reliable manner, how can we reach a balance between our ability to measure and our assessment of the environmental risk? Robert M. White, president of the National Academy of Engineering, recently stated that the impact of technological innovation can lead to a greater ability to detect and analyze, or it can bring about wholly new processes or products (18).The new analytical understanding helps in the development of processing changes to lower emissions or contaminants. He argues in a very persuasive analysis that “There is a cyclical nature to the evolution of technology and the environmental c h a11e nge s we face -technology shapes society and society shapes technology.” An example is in the history of lead pollution. The presence of lead in air and water was the result of the burning of coal; the metallurgical indus-
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try; and, after World War 11, gasoline use in automobiles. The toxic effects of lead were well documented long before 1970, when the Clean Water Act initiated action on determining harmfid levels and regulating lead. But links between human activities, environmental lead contamination,
and ecological effects had to await more sensitive detection limits. Figure 5 shows the dramatic improvement in our analytical capabilities for lead determination in water. As our ability to quantitatively detect and measure lead improved, society responded with technological innova-
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Figure 4. GC/FT-IR determination of aldehydes in municipal effluent. (Adapted with permission from Reference 16.)
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Figure 5. Detection limits for lead in routine water quality measurements from 1955 to 1990. Dotted line represents federal guidelines for lead in fresh water, 3.2 pg/L.
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REPORT tions to replace lead-for example, unleaded gasoline; substitutes for lead-based paints; replacement material for lead water pipes; and alternatives to lead solder, including seamless aluminum cans. The cycle of awareness, social response, and technological innovation was predi cated on our ability to determine lead in smaller amounts in complex samples.
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Process control Analytical chemistry has been at l e a s t p a r t i a l l y r e s p o n s i b l e for changes i n t h e philosophical a p proach of industry in addressing environmental problems. Because the United States spends $116 billion annually (2.1% of the GNP) on environmental improvements (19),the impact of our ability to measure reliably can be enormous. The evolutionary response of corporations to environmental issues has been characterized by an EPA official as “from pollution control to waste management to waste minimization to pollution prevention’’ (17). The technology that has been the spearhead of this change is a new generation of sophisticated, but rugged, instruments that can be used in line, not only on line, to monitor process operations (20). Process control, quality control, and quality assurance have become the new frontiers of analytical science. Such advanced techniques as FT-IR, X-ray fluorescence, and flow injection analysis are being used to enhance profitability while simultaneously allowing operating manage ment to reduce emissions and waste. Key to these new applications are startling developments in microelectronics, fiber optics, and chemomet ric data handling (21).Nearly all major chemical companies can relate instances i n t h e i r operations i n which sophisticated process analytical instrumentation has led to increased competitiveness and significant contributions to proactively enhancing environmental protection. Published data from NIST put the case in perspective, as shown in the box above. Measurement -related activity is estimated to comprise 3.5% of the gross national product in the United States. The cost to industry for such measurements is $50 billion per year, and 250 million measurements per day are made with a retest rate as high as 30%. If, through process control by advanced analytical technology, this retest rate could be dropped to 5%, the estimated cost saving in U.S. manufacturing would be 20%.
ANALYTICAL CHEMISTRY, VOL. 64, NO. 13, JULY 1,1992
conomic impac materials r asure
Proactive efforts by chemical companies to reduce environmental pres sures by a variety of methods are making progress. In addition, chemical companies that are members of the Chemical Manufacturers Association have adopted a new program called Responsible Care (22). It consists of a set of Guiding Principles and six Codes of Management Practices to put the Guiding Principles into action. The Guiding Principles are listed below. Be safe and environmentally responsible in the manufacture, trans portation, storage, use, and disposal of chemicals. Respond to community concerns about chemicals and operations. Help communities put emergency procedures in place to handle spills and other releases-procedures that also can be useful in responding to natural disasters. Keep the public and government officials informed about chemicalrelated health and environmental hazards. The companies should be commended for these challenging objectives and for positive action. Conclusion Is analytical chemistry feeding the environmental revolution? I believe that we know only what we can measure. The answer lies not in slowing down our search for analytical understanding, but in intensifying it. This search must be coupled with increased efforts to present the information obtained in terms the audience can understand. Overall, a n honest portrayal of risk, on a scientific basis, should be the goal of industrial and academic scientists, and the aim of industry should be to drive this exposure to a n absolute minimum. But we will know that we are at that minimum only with state-of-
the-art analytical science. In matters of environmental concern, analytical chemistry will be the solution, not the problem. Much of the substance of this paper came from work published and presented over the years by the late L. B. Rogers, who was Emeritus Professor at the University of Georgia. In particular, his work as chair of the ACS Division of Analytical Chemistry’s Subcommittee for Public Awareness resulted in a paper presented at the Atlanta ACS meeting in April 1991 from which I have abstracted many thoughts. I a m deeply grateful to Buck for sharing his wisdom and perceptions with me.
I would also like to thank Tim Collette, Bill Donaldson, and Don Gurka from t h e EPA, Harry Hertz from NIST, and Cliff Narquis from BP Research for helpful information and discussions.
References (1)Grasselli, J. G. In Analytical Applications of Spectroscopy ZI; Davies, A.M.C.; Creaser, C. S., Eds.; The Royal Society of Chemistry: Cambridge, U.K., 1991. (2)Hertz, H. S.Anal. Chem. 1988,60,76A. (3) Pimentel, G. “Opportunities in Chemistry,” National Academy of Sciences: Washington, DC, 1985. (4)Collette, T. W., EPA, personal communication, Aug. 1991.
(5) Donaldson, W. T., EPA, personal communication, Aug. 1991. (6)Roberts, L. Science 1990,249,616. (7)Covello, V.T. Environ. Sci. Technol. 1989,23,1444. (8)Baker, J. K. Anal. Chem. 1991, 63, 779 A. (9)Wilson, R.; Crouch, E.A.C. In Cancer Risk Assessment; Travis, C. C., Ed.; Plenum: New York, 1988;p. 183. (10)Rogers, L.B. Presented at the National Meeting of the American Chemical Society, Atlanta, GA, April 1991. (11)Rogers, L.B. CHEMTECH 1991, 21(4),229. (12)Cinman, B. D. Science 1972, 174, 495. (13)h e s , B. N.; Gold, L. S. Chem. Eng. News Jan. 7, 1991,p. 28. (14)Travis, C. C.; Hattemer-Frey, H. A. Environ. Sci. Technol. 1988,22,873. (15) Stanko, G. H.; Hewitt, R. W. Presented at the 12th Annual EPA Conference on Analysis of Pollutants in the Environment, Norfolk, VA, May 1989. (16)Richardson, S.D.; Thurston, A. D., Jr.; Collette, T. W.; McGuire, J. M. Environ. Toxicol. Chem. 1991,10,991. (17)Gurka, D. F.,EPA, personal communication, Aug. 1991. (18)White, R. M.; Rod, S. R. Environ. Sci. Technol. 1990,24,460. (19) Corporate Environmental Management, A n Executive Survey; Booz-Allen a n d Hamilton: Bethesda, MD, 1991. (20)Callis, J. B.;Illman, D. L.; Kowalski, B. R. Anal. Chem. 1987,59,624A. (21)Turner, S.; Steel, E. B. Anal. Chem. 1991,63,868.
I From Caveman to Chemist I Circumstancesand Achieve
Responsible Ca re -Progress Report , Chemical Manufacturers Association: Washington, DC, 1991.
( 22)
Jeannette G. Grasselli is a Distinguished Visiting Professor and Director of Research Enhancement at Ohio University. Previously she was a research director in BP America’s R&D department. She received her B.S. degree in chemistry from Ohio University and her M.S. degree from Case Western Reserve University. She has also received honorary DSc. degreesfrom Ohio University (1978) and Clarkson University (1986) as well as an honorary D.Engr. degree from Michigan Technological University (1989). In 1986she received the ACS Garvan Medal, and in 1991 she was the first woman elected to the Ohio Science and Technology Hall of Fame.
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