Chemical & Engineering News 1155— 16th St., N.W., Washington, D.C. 20036 Editor: Michael Heylin Managing Editor: William F. Fallwell Assistant Managing Editors: David M. Kiefer, James H. Krieger, Donald J. Soisson Staff Editor: Ernest L. Carpenter Senior Editors: Earl V. Anderson (New York), Lois R. Ember, Wilbert C. Lepkowski, Howard J. Sanders Associate Editors: Doron Dagani, Rebecca L. Rawls, Richard J. Seltzer Assistant Editors: Mairin B. Brennan, Pamela S. Zurer Editorial Assistant: Theresa L. Rome Editing Services: Joyce A. Richards (Head), Dolores Miner (Editorial Assistant) News Bureaus: New York: (212) 697-3223 William J. Storck (Business Editor), Stephen C. Stinson and David Webber (Associate Editors). Chicago: (312) 236-7325 Ward Worthy (Head), Joseph Haggin (Associate Editor). Houston: (713) 973-8161 Bruce Γ. Greek (Head). Washington: (202) 872-4496 Janice R. Long (Government Editor), David J. Hanson (Associate Editor). West Coast: (415) 665-4971 Rudv M. Baum (Head). Foreign Bureau: London: (0Î) 540-0414 Dermot A. O'Sullivan (Head) and Patricia L. Layman (Associate Editor) Indexer: Nancy R. Gleboff Graphics and Production: Elmer M. Pusey Jr. (Head). Leroy Corcoran (Manager). Alan Kahan (Art Director). Barbara Haves (Designer). Linda Mattinglv (Staff Artist). Diane K. Lilienkamp (Costing). Business Manager: Arthur Poulos Circulation Development: Cynthia G. Smith ADVISORY BOARD: Robert A. Alberty, William O. Baker, John D. Baldeschwieler, EulaBingham, William A. Blanpied, John I. Brauman, George E. Brown Jr., John M. Deutch, Catherine Fenselau, Mary Good, S. Allen Heininger, James D. Idol Jr., Ray R. Irani, Peter J. Lucchesi, Kurt Mislow, George C. Pimentel, Bryant W. Rossiter Published bv AMERICAN CHEMICAL SOCIETY (202) 872-4600 John Κ Crum, Executive Director EDITORIAL BOARD: John G Verkade (Chair man); Board of Directors Chairman: Clayton F. Callis; President-Elect: Warren D. Niederhauser; Immediate Past-President: Robert W. Parry; VVendell L. Dilling; Richard M. Lemmon; John H. Nelson; and Louis D. Quin. © Copyright 1983, American Chemical Society Subscription Service: Send all new and renewal subscriptions with payment to: Director of Finan cial Operations, ACS, 1155—16th St., N.W., Washington, D.C. 20036. Correspondence and telephone calls for changes of address, claims for missing issues, subscription service, status of rec ords and accounts should be directed to: Manager, Membership & Subscription Services, ACS, P.O. Box 3337, Columbus, Ohio 43210; (614) 421-3776. Changes of Address: Include both old and new addresses with ZIP code numbers and mailing label from a recent issue. Allow four weeks for change to become effective. Claims for missing numbers will not be allowed if loss was due to failure of notice of change of address to be received in the time specified; if claim is dated (a) North America, more than 90 days beyond issue date, (b) all other foreign; more than one year beyond issue date; or if the reason given is "missing from files." Subscription Rates 1983. Printed or microfiche editions: nonmembers U.S. 1 yr. $34, 2 yr. $64; outside U.S. 1 yr. $58, 2 yr. $112. Air freight rates available on request. Rates above do not apply to nonmember subscribers in Japan, who must enter subscription orders with Maruzen Co. Ltd., 3-10 Nihonbashi 2-chome, Chuo-ku, Tokyo 103, Japan. Tel: (03) 272-7211. Single copies: Current $2.00. Rates for back issues and volumes are available from Distribution Office, ACS, 1155—16th St., N.W., Washington, D.C. 20036. An annual index is available for $35 at the same address. Back and current issues available on microfilm and micro fiche. Contact Microform Program, ACS. Chemical & Engineering News (ISSN 0009-2347) is published weekly except for the last week in December by the American Chemical Society at 1155—16th St., N.W., Washington, D.C. 20036. Second class postage paid at Washington, D.C, and additional mailing offices. POSTMASTER: Send address changes to Membership & Subscription Services, P.O. Box 3337, Columbus, Ohio 43210. ACS assumes no responsibility for the statements and opinions advanced by the contributors to its publications. Advertising Management CENTCOM LTD. (For list of offices see page 85) 4
December 5, 1983 C&EN
LETTERS
CHEMICAL SAFETY Tragic consequence with acetonitrile adduct SIR: I would like to bring to your attention an extremely hazardous material which may re sult from a relatively small change in the procedure of a published preparation. The compound in question is an acetonitrile adduct of neodymium perchlorate. In the preparation of a neodymium amine complex we have previously reported the use of the anhydrous acetonitrile adduct, Nd(C10 4 )3-4CH 3 CN as an intermediate [Eigenbrot and Raymond, hwrg. Chem., 21, 2867 (1982)]. This preparation followed a procedure used by Johnson and Forsberg (Inorg. Chem., 15,734 (1976)) in which the neodymium perchlorate is dissolved in acetonitrile and the amine is added to this solution. The extraction of the perchlorate with acetonitrile allows the sepa ration of the anhydrous perchlorate from the oxide and other impurities [Forsberg et al., hwr$. Chem., 10, 2656, (1971)]. Evaporation of the acetonitrile solution under vacuum at room temperature gives the compound whose composition is Nd(OC>4)3· 4CH 3 CN. Routine handling of this material has indicated that it has no unusual thermal or shock sensitivity. In contrast, drying of the acetonitrile adduct at 80° under vacuum pro duces a compound whose apparent composi tion is the bis(acetonitrile) adduct, Nd(C10 4 )3-2CH 3 CN, and which can detonate on contact. On Aug. 10, Jean-René Hamon, a visiting postdoctoral research scientist from the C.N.R.S. Laboratories in Rennes, France, apparently prepared the bis(acetonitrile) adduct when he dried the residue from the acetonitrile solution at 80 ° C A small amount (on the order of a gram) exploded in a cylindrical flask
which he was holding in his left hand. What is most unfortunate, Hamon had just removed his safety glasses to wipe perspiration from his face and eyes when the explosion occurred. The actual magnitude of the explosion was not great, but it has caused terribly serious injuries to Hamon. He lost the small and ring finger of his left hand. Much worse, he has lost his right eye and the left eye is seriously injured. What is doubly tragic is that essentially the same compound was prepared by Wayne C. Wolsey. In his case it was the dried Er(C104)3· 4CH 3 CN salt which detonated on scraping with a spatula, resulting in the loss of one finger and injury to a second. Wolsey then wrote an article about this [/. Chew. Ed., 50, A355 (1978)] which was brought to my attention by Leslie Bretherick after Hamon's accident. I and my research group were unaware of the Wolsey article, as apparently was Forsberg, since his 1976 article does not cite it. The scenario described by Wolsey appears to be essentially the same as that followed by Hamon. Hamon was developing procedures to substitute the trifluoromethyl sulfonate (triflate) anion for perchlorate in following the synthetic procedures that have been used in manufacturing a number of anhydrous lanthanide amine complexes. In general, when noncoordinating agents are required, every attempt should be made to substitute anions such as triflate for perchlorate. If a perchlorate must be used, only small amounts of material should be prepared and they should be handled with adequate caution. Kenneth N. Raymond Professor of Chemistry University of California, Berkeley
VA registrants exposed to agent orange SIR: A recent correspondent (Letters, C&EN, Nov. 7, page 2) contrasts his calculated incidence rate of 7.06 per 100,000 for soft-tissue sarcoma (STS) among 42,500 exposed Vietnam veterans, listed in the Veterans Administration Agent Orange Registry, with a figure of 12.89 quoted in an earlier article. Both figures are meaningless. Incidence is the rate of occurrence of a disease in a population during a specific time interval, whereas observations were made on these men at a single time only. No information currently available about this registry group can provide the basis for either
an incidence or mortality calculation. At best, one might calculate the prevalence rate (number of cases divided by population), but this biased figure would reflect little more than the relative propensity of ill persons to present themselves for registration, and would be irrelevant to the relationship between exposure to agent orange, or to anything else, and disease. Furthermore, even if it could be shown that 42,500 registrants were exposed to agent orange and an equal number unexposed, the Continued on page 84
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Continued from page 4 prevalence of STS is so small that at least 10 of the 11 STS cases would have to fall into the exposed group to yield a significant difference at the 5% level. If the relative risk were less than 5:1, a hefty risk for any type of cancer, there would be insufficient statistical power to achieve significance, and a statistical com parison of STS prevalence between the ex posed and unexposed groups would be pointless. The registry group will be useful only if traced into the future, and new cases of cancer accurately identified. Even so, the incidence rate of STS is so low that in a group of 42,500 men having the age distribution of Vietnam war veterans, only about 0.7 new case of STS per year would be expected, based upon NCI SEER Program figures for 1973-77, which are the best now available. Thus, in the total reg istry group of 83,000, we expect to see no more than seven new cases occurring in the next five years, based upon these rates. Again, un less, the latency of agent orange is shorter and its carcinogenic effect greater than prac tically any known carcinogen, this population is too young and too few in number to make an STS study worthwhile.
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Finally, even if such a study were under taken, actual observation of new cases depends upon the VA's accurately determining the health status of every single one of these men year after year. During the September ACS meeting, Barclay Shepard of the VA's Agent Orange Projects Office told the Dioxin Sym posium that this registry could provide a mechanism for such followup in the future, but that none is scheduled so far. For the mo ment, the relation between agent orange ex posure and STS in these 83,000 men remains a matter of speculation only. Steven D. Stellman Assistant Vice President for Epidemiology American Cancer Society Jeanne M. Stellman Associate Professor of Public Health Assistant Director, Comprehensive Cancer Center Columbia University
Sexipyridine synthesis SIR: The publication of the synthesis of a "sexipyridine" by George R. Newkome and H.-W. Lee [/. Am. Chem. Soc, 105,5956 (1983)] was described in the Science/Technology Concentrates of the Sept. 19 issue of C&EN. Although this represents the first synthesis of an unsubstituted // sexipyridine, ,, the first "sexipyridine" synthesis was reported by John L. Toner of Eastman Kodak Co. [Tetrahedron Lett., 2707 (1983)]. Michael R. Detty Chemistry Division Research Laboratories, Eastman Kodak Rochester, Ν. Υ.
