Newscripts
by Κ. Μ. Reese
A familiar phrase C&EN's man in Tokyo notes that with all the Japanese delegations flocking to China nowadays, a phrase is becoming current in Japan that has a familiar ring. It occurs in this recent conversational exchange in Tokyo: Speaker A: "Oh, so Mr. Y is in China! Has he been there before?" Speaker B: "Yes . . . during the war."
Deep countercurrent measured in Gulf Stream The surface flow of the Gulf Stream through the Florida Straits is generally northward, but research by scientists at the University of Miami suggests that up to 20% of the entire water flow through the straits is sometimes moving south. Scientists have suspected for decades that a countercur rent might exist beneath the Gulf Stream's
Letters Words on birds SIRS: Your editorial (15 May), Which quoted letters quite reproving, Described not ostrich but the jay Which cries alarm at all things moving. The jays prefer the status quo, And flock together for protection. Well-feathered nests some owls can show From silent swoops and skilled selection. One full-fledged cardinal rule I follow: Don't be egged on or gulled too much By hawkers whistling in the dark. Conformity is hard to swallow If chosen blindly in the clutch, Too swiftly, or just for a lark. Richard K. Putneyι Hudson Falls, N.Y. SIRS: May I take exception to your edi torial of May 15—"Of swans, ducks, and1 ostriches"? We "enlightened elite" should maintain our beliefs, knowledge, and wisdom, and not be distracted by theι "rabble." All opposition should be sup pressed. C&EN should be a m o n o l i t h no room for divergent opinions. How/ else can we educate the " m a s s e s " in theι " t r u e word"? To do otherwise is to allow a wedgeι for democracy to creep in, and all wes "elite authoritarians" know the folly off democracy—be it in politics or ACS. With tongue in cheek, Cincinnati, Ohio Henry R. Greeb3 SIRS: I commend Patrick P. McCurdy, and wholeheartedly support his edi torial views in the May 15 C&EN. Thes expression of his ideas could not havee been more timely than in the wake off another tragedy in our political arena; the abhorrent results of intolerance. The fear of opposing views seems to be ae characteristic of individuals whose ownaι views are based on very weak foundationss indeed. Joseph K. Valaitiss May field Heights, Ohio 42 C&EN JUNE 12, 1972
surface flow. The question remained un resolved, however, because of the lack of means for measuring current in the diffi cult conditions in the straits. The means is now available in the form of a profiling current meter developed by Dr. Walter Duing and his colleagues at the university's Rosenstiel School of Marine and Atmos pheric Science. The meter is attached to a wire sus pended beneath an anchored ship and descends slowly through the water column. Data on current speed and direction, tem perature, pressure, and salinity are re corded on magnetic tape as the instrument sinks. Dr. Duing and his associates are using the equipment in a large-scale study of the dynamics of the Gulf Stream. Computer analyses are being made of more than 500,000 readings taken by four ships over a period of 16 days. These are the data that suggest the existence of the south ward flow, which evidently occurs mainly in the deep parts of the western side of the Florida Straits. The flow appears to occur
once or twice a week in "spurts" that last about two days. Dr. Duing's data also indicate east-west meandering of the current axis at the sur face of the straits. An effort will be made to determine if the meanders occur in pre dictable cycles. If they do, the knowledge could save hours of steaming time for ships that pass through the Florida Straits.
SIRS: Your May 15 editorial was very appropriate. I applaud your decision to invite Mr. Mazzocchi to write his editorial, and hope you include other strongly held opinions in future issues. We can learn much from an honest advocate. Pseudoobjectivity is not a desirable trait. Lancaster, Pa. F. Melvin Sweeney
" n u r t u r e d this gleam of an idea before it became a goal." Now, with so many scientists out of work, this sort of retracking may give them something to fall back on, so to say, when their wives get tired of having them around the house all day. Robert Romaine Air Pollution Fellow, Drexel University, Philadelphia, Pa.
Council measures SIRS: The news story (C&EN, April 24 page 27) summarizing ACS Board and Council activities at the Boston meeting constituted, I thought, a good summary. However, two important items were omit ted: 1. The Council passed a revision in the requirements for ACS membership, al though, as you reported, leaving the asso ciate membership category untouched. The details of the revision are compli cated, but their main content is to ease membership requirements for chemists who obtained their degrees in "closely related sciences," such as biochemistry, chemical physics, etc. Previously, except for provisions of a "significant achievem e n t " clause, the applicant for member ship had to have a degree in chemistry or chemical engineering. 2. The Council also passed a very limited subsidy for the travel expenses of councilors to national meetings. The national ACS subsidy must be matched by equal amounts from the local sections and divisions (more than 30 local sections al ready subsidize their councilors' travel expenses). It is hoped that this plan will make service on the Council more avail able to younger members and members from small research organizations. Richard M. Lemmon Councilor, California Section, Berkeley, Calif.
Teacher's comment SIRS: I found Aram H. Sevagian's com· ment (C&EN, May 1, pages 22 and 30) on David B. Sabine's statement (C&EN, March 20, page 49) very interesting, Yes, it was my high school teacher's comment on homo genine reactions that
Department of obscure information • Canada produced 46.7 million troy ounces of silver last year. • The U.S. produces 5 to 6 billion pounds of beef fat annually. • 25,125 veterinarians were practicing in the U.S. as of Jan. 1, 1970. • The water frozen in the Antarctic ice cap would feed the Mississippi River for more than 50,000 years. • Modern pewter contains up to 97% tin with small amounts of antimony and copper. • Natural rubber accounts for 42% of Malaysia's foreign exchange.
Hazards of carbon monoxide in cylinders SIRS: Carbon monoxide gas in cylinders is used either alone or in conjunction with other gases for many industrial and research purposes. Users of this gas are normally acquainted with its inherent toxicity, but through recent experiences at our laboratory we have been made aware of additional dangers that may be less well recognized. We uncovered these hazards during an experiment in which flowing carbon mon oxide from a commercially vended cylinder was used as a reducing agent in a furnace heated at 500° C. for 24 hours. On opening the furnace, we observed de posits of carbon and iron on the platinum heating element and on the specimen which was the subject of our experiment. Our findings led us to study available data on possible reactions between CO and the materials in which it may b e contained, and to carry out additional tests. The following paragraphs briefly describe the results of our efforts. The source of iron in our experiment was traced to the presence of iron pentacarbonyl in the carbon monoxide gas stream. Smaller amounts of nickel tetracarbonyl were also detected. Formation of the carbonyls in the cylinder is due to a reaction of CO on the steel cylinder wall. Few users of the gas appear to be aware of this reaction even though the chemical literature contains references to its occurrence. One such report (1) showed iron pentacarbonyl contents vary ing from 0.16 to 18 mg. per liter in samplings from a group of carbon mon oxide gas cylinders. Continued on page 33
LETTERS
Continued from page 42
Though there is no dispute as to the presence of carbonyl compounds in car bon monoxide gas cylinders, the cause of their formation is not thoroughly under stood. The original synthesis of Fe(CO).-, by Mond and Quinke (2) was effected by reacting CO at atmospheric pressure and 80° C. with an active form of iron metal. Increases in gas pressure and tempera ture were observed to improve the carbonyl yield. The rate of formation and the quantity of Fe(CO) r) were sig nificantly increased by use of sulfur, selenium, or tellurium catalysts (3). Sup pliers of commercial carbon monoxide have suggested sulfur in steel as the cause of carbonyl generation in their cylinders and have proposed its removal as a means of stopping the reaction. Evidently little has been done to p u t this proposal into effect. A decrease in tank pressure has also been proposed to lower the rate of carbonyl formation. In 1957 the Oak Ridge Gaseous Diffusion Plant adopted a procedure for the pur chase of CO in cylinders that required tank pressures to be no greater than 1000 p.s.i. As noted below, most commercial \ r endors of the gas normally exceed this fill pressure. Of the four carbon monoxide cylinders examined in our tests, two had been in our laboratory for more than two years, while two had been recently purchased. Both older cvlinders contained about 24 p.p.m. (0.2 mg. per liter) of Fe(CO)r>; the newer cylinders were apparently uncontaminated. All four cylinders were de livered at tank pressures of 1500 p.s.i. From this admittedly limited sample, we
suggest that storage of filled CO cylinders for periods of a year or more will prob ably result in formation of demonstrable quantities of carbonyl compounds. The dangers associated with this carbonyl formation are twofold: first, the synthesis of unexpected toxic gases; and second, the corrosion of the gas cylinder. As noted above, careful analyses of our gases revealed not only Fe(CO)-, but, more importantly, Ni(CO) t for which the toxic threshold is only 1 p.p.b. (4). It was in structive to find 15 p.p.m. (0.01 mg. per liter) of this nickel compound in the gas from one of our cylinders. One may be tempted to dismiss so small an amount of a secondary toxic gas in the presence of so great an amount of toxic CO. Dif ferences in the physical and chemical properties of the two compounds could, however, lead to a segregation and ac cumulation of the highly persistent nickel tetracarbonyl that might present an un expected danger, for example, in the neighborhood of an exhaust system. The second danger arises from the structural degradation of the gas cylinder itself. Eventual cracking may be ex pected as the corrosion process con tinues and catastrophic failures of the cylinder walls have indeed been reported (5). One may also speculate on the con sequences of refilling partially corroded cylinders at CO pressures normally em ployed by the commercial vendor. Finally, apart from the question of safety, the chemical effects that the carbonyl contaminants may have in a given experiment or process must be considered. Materials heated in a carbonyl-contaminated CO atmosphere
(1) J. Sendroy, Jr., H. A. Collison, and H. J. Mark, "Determination of Iron Pentacarbonyl in Commercial Carbon Monoxide," Anal. Chem., 1641 (1955). (2) L. Mond and F. Quinke, "Note on a Volatile Compound of Iron with Car bonic Oxide," J. Chem. Soc. London, 604 (1891). (3) W. Hieber and O. Geisenberger, "Uber den Einflus con Chalkogenen auf Continued on page 41
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may easily acquire significant amounts of carbon and transition metal impurities through decomposition of the carbonyls. Further reactions of these elements with the normal components of the experiment may follow. We conclude that users of commercially purchased cylinders of carbon monoxide should: (a) Store these cylinders for the mini m u m possible time. (b) Routinely provide means by which carbonyls in the gas may be entrapped before reaching critical parts of the ex periment or process. (c) If (b) is not followed, use extra care in venting the gas to the atmosphere. We also suggest that suppliers of carbon monoxide should: (a) Initiate real efforts to decrease the rate of carbonyl-forming reactions by lowering tank pressures and by using special steels in cylinder construction. (b) Develop tests to determine the presence and extent of corrosion in cylinders returned for refilling, using re sults of these tests to set maximum tolerable limits for the future use of the cylinder.
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e)
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OPTICALLY ACTIVE ALCOHOLS 2-Butanol through 2-Octanol ( + ) and (—) isomers available
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INTERFACE
CO * All the Elements * Valence Shifts * Top 100 Angstroms
RESEARCH
ACETYLENIC CHEMICALS
ESCA * Fractions of a Monolayer * Surface Contaminants * Profiles of Multilayers
(415) 968-0375*P.O. Box 1088 Mtn View Ca 94040
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INDEX TO ADVERTISERS IN THIS ISSUE AQUITAINE 9 Serma ARCO Chemical Company, Petrochemical Dept IFC Lennen & Newell, Inc. BASF Wyandotte Corporation 4 Ross Roy Inc. Diamond Shamrock Chemical Company, Intermediate Chemicals Div 32 Meldrum and Fewsmith, Inc. *Ethyl Corporation 7 Gaynor & Ducas, Inc. GAF Corporation, (PVP Derivatives) IBC Michel-Cather, Inc. Jefferson Chemical Company 12 Robinson-Gerrard/Inc. *Pfizer, Inc OBC D'Arcy-MacManus-Intermarco, Inc. Rohm and Haas Company 15 APCL&K Inc. Schweiz;Sprenstoffabrik 28 Publicitas Service International DIRECTORIES Chemicals Exchange 33 Classified Advertising 34-40 Technical Services 33
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LETTERS Continued
|
from page 33
die Entstehung von Eisenpentacarbonyl aus den Komponenten," Z. Anorg. Allg. Chem., 262, 15 (1950). (4) Hygienic Guide Series, American Industrial Hygiene Association, May-June 1968. (5) (a) Process Safety Department, Memorandum 795, Carbide and Carbon Chemicals Co., South Charleston, W.Va. (b) A. L. Mossman, Matheson Co., Inc., private communication. L. A. Harris and H. L. Yakel Metals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, Tenn. SIRS: Thank you for the opportunity to comment on the correspondence from L. A. Harris and H. L. Yakel. Our company produces metal carbonyls and we utilize carbon monoxide in cylinders and cylinder-trailers. We also produce nickel carbonyl in commercial quantities. Our general reaction to the above report is one of approbation and a feeling that it should be published to inform others that carbon monoxide (or any reagent) may contain impurities; that these impurities may affect the results of experiments; and that in this particular case, these impurities may be toxic. Republication of literature references to alert again users of carbon monoxide in cylinders to these problems should be useful. The laboratory and chemists using the gas certainly must assume some responsibilities. In one case (5) the cylinder which gave some difficulty had been kept at the laboratory for many years— long enough to prevent the gas supplier from performing the periodic inspection required. However, one incident resulted in strict controls to prevent such long storage. One interesting economic control which might force the chemist to return a cylinder after one year could be a very large increase in cylinder rental charges after a one-year period. Any reaction requiring high reagent purity usually necessitates purification of any purchased commodity. While most of us would normally recrystallize a solid and redistill a liquid, there seems to be a blind spot regarding compressed gases. These should be treated as any other reagent and purified before being introduced in the reaction scheme. We urge the careful researcher to do so regardless of the purity supposedly guaranteed by the supplier. Finally, while the metal carbonyls are more toxic in many cases than carbon monoxide, they are not unknown materials and uhey are handled in large quantities. For both iron pentacarbonyl and nickel tetracarbonyl, there are established allowable levels and handling procedures. I find it hard to believe that the nickel carbonyl was formed in the carbon monoxide cylinder. This compound could have been formed in some external system and reintroduced to the cylinder by the user or could have been produced in the analytical procedure used. We agree that any user of carbon monoxide should be alerted to the probability of finding iron pentacarbonyl as a contaminant but we cannot agree that nickel tetracarbonyl can be considered a normal contaminant of cylinder carbon monoxide without more data. E. L. Clark President, Pressure Chemical Co., Pittsburgh, Pa.
RECENTag§ MONOGRAPHS COORDINATION CHEMISTRY Volume I Edited by Arthur E. Martell. ACS 168. Just published. A study of physical and chemical properties of metal complexes. Provides a perceptive account of the reaction mechanisms that these complexes undergo. The book covers many subjects of special interest, including Mossbauer spectroscopy, mixed ligand complexes, metalmetal bonds, interpretation of Xray crystallography, and important changes in areas such as nuclear magnetic resonance and electron spin resonance. 578 pp., 153 illus., $32.50.
ISOTOPE EFFECTS IN CHEMICAL REACTIONS Edited by Clair J. Collins and Newell S. Bowman. ACS 167. Examines the mechanistic use of kinetic isotope effects and the deductions drawn from isotope-effect data. Describes the meaning and use of heavy atom isotope effects as applied to chemical research, isotope effects in biological systems and on aliphatic nucleophilic substitution reactions, and the relationship between "neighboring group participation" and secondary isotope effects of deuterium. 436 pp., illus., $22.50.
BACTERIOPHAGE BIOCHEMISTRY Christopher K. Mathews. ACS 166. An in-depth review of the biochemistry of bacterial viruses, emphasizing metabolism of virus-infected cells. Presents supporting information in related areas of phage structure, viral genetics and microbial physiology. Includes significant data and results in areas such as T-odd phages, temperate phages, single-stranded DNA phages, and bacullus subtilis phages. 382 pp., illus., $19.95. 10-DAY FREE EXAMINATION
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JUNE 12, 1972 C&EN
41
LETTERS
Continued from page 42
Though there is no dispute as to the presence of carbonyl compounds in car bon monoxide gas cylinders, the cause of their formation is not thoroughly under stood. The original synthesis of Fe(CO).-, by Mond and Quinke (2) was effected by reacting CO at atmospheric pressure and 80° C. with an active form of iron metal. Increases in gas pressure and tempera ture were observed to improve the carbonyl yield. The rate of formation and the quantity of Fe(CO) r) were sig nificantly increased by use of sulfur, selenium, or tellurium catalysts (3). Sup pliers of commercial carbon monoxide have suggested sulfur in steel as the cause of carbonyl generation in their cylinders and have proposed its removal as a means of stopping the reaction. Evidently little has been done to p u t this proposal into effect. A decrease in tank pressure has also been proposed to lower the rate of carbonyl formation. In 1957 the Oak Ridge Gaseous Diffusion Plant adopted a procedure for the pur chase of CO in cylinders that required tank pressures to be no greater than 1000 p.s.i. As noted below, most commercial \ r endors of the gas normally exceed this fill pressure. Of the four carbon monoxide cylinders examined in our tests, two had been in our laboratory for more than two years, while two had been recently purchased. Both older cvlinders contained about 24 p.p.m. (0.2 mg. per liter) of Fe(CO)r>; the newer cylinders were apparently uncontaminated. All four cylinders were de livered at tank pressures of 1500 p.s.i. From this admittedly limited sample, we
suggest that storage of filled CO cylinders for periods of a year or more will prob ably result in formation of demonstrable quantities of carbonyl compounds. The dangers associated with this carbonyl formation are twofold: first, the synthesis of unexpected toxic gases; and second, the corrosion of the gas cylinder. As noted above, careful analyses of our gases revealed not only Fe(CO)-, but, more importantly, Ni(CO) t for which the toxic threshold is only 1 p.p.b. (4). It was in structive to find 15 p.p.m. (0.01 mg. per liter) of this nickel compound in the gas from one of our cylinders. One may be tempted to dismiss so small an amount of a secondary toxic gas in the presence of so great an amount of toxic CO. Dif ferences in the physical and chemical properties of the two compounds could, however, lead to a segregation and ac cumulation of the highly persistent nickel tetracarbonyl that might present an un expected danger, for example, in the neighborhood of an exhaust system. The second danger arises from the structural degradation of the gas cylinder itself. Eventual cracking may be ex pected as the corrosion process con tinues and catastrophic failures of the cylinder walls have indeed been reported (5). One may also speculate on the con sequences of refilling partially corroded cylinders at CO pressures normally em ployed by the commercial vendor. Finally, apart from the question of safety, the chemical effects that the carbonyl contaminants may have in a given experiment or process must be considered. Materials heated in a carbonyl-contaminated CO atmosphere
(1) J. Sendroy, Jr., H. A. Collison, and H. J. Mark, "Determination of Iron Pentacarbonyl in Commercial Carbon Monoxide," Anal. Chem., 1641 (1955). (2) L. Mond and F. Quinke, "Note on a Volatile Compound of Iron with Car bonic Oxide," J. Chem. Soc. London, 604 (1891). (3) W. Hieber and O. Geisenberger, "Uber den Einflus con Chalkogenen auf Continued on page 41
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may easily acquire significant amounts of carbon and transition metal impurities through decomposition of the carbonyls. Further reactions of these elements with the normal components of the experiment may follow. We conclude that users of commercially purchased cylinders of carbon monoxide should: (a) Store these cylinders for the mini m u m possible time. (b) Routinely provide means by which carbonyls in the gas may be entrapped before reaching critical parts of the ex periment or process. (c) If (b) is not followed, use extra care in venting the gas to the atmosphere. We also suggest that suppliers of carbon monoxide should: (a) Initiate real efforts to decrease the rate of carbonyl-forming reactions by lowering tank pressures and by using special steels in cylinder construction. (b) Develop tests to determine the presence and extent of corrosion in cylinders returned for refilling, using re sults of these tests to set maximum tolerable limits for the future use of the cylinder.
BURDICK & JACKSON LABORATORIES INC.
Advertising Rates: Space rate is $94 per inch. Lower rates available on contract basis. An "inch" ad vertisement measures %" deep on one column. Additional space in even lineal inch units. Maximum space—4" per Directory per issue. Set ads due 21 days in advance of publications; plated ads, 17 days.
e)
n
fyt. \ —
/
NH.
D(+)/*ZW/J-METHYLBENZYL AMINE MUSKEGON. MICHIGAN 4 9 4 4 2
Potassium-tert-butylalcoholate Alcohol-free dry powder
TECHNICAL SERVICES
Now available in commercial quantities
MSA RESEARCH CORP.
Moving? SEND FOR BOOKLET A free 32-page booklet prepared by Burnham Van Service, Inc., can give you helpful work-saving, cost-saving pointers on how to organize your move from city to city when you change jobs. How to prepare to move, tips on packing, a helpful inventory check list of things to do are among the topics included. Write for your free copy. No obligation. Miss Patricia Flynn Burnham Van Service 1634 Second Avenue Columbus, Georgia 31091
SCHWARZKOPF MICROANALYTICAL LABORATORY
STEREOISOMERS
56-19 37th Ave., Woodside, N.Y. 11377 Telephone: Code: 212, HAvemeyer 9-6248, 9-6223 ELEMENTAL ANALYSES ORGANICS, INORGANICS, ORGANO METALLICS METALS BY ATOMIC ABSORPTION MOLECULAR WEIGHT, FUNCTIONAL GROUP Trace Analyses Research
Routine
analyses
within
Evans City, Pa. 16033
OPTICALLY ACTIVE ALCOHOLS 2-Butanol through 2-Octanol ( + ) and (—) isomers available
5 days
^ÎORSl
I NORSE LABORATORIES INC.] AITV κι H
LOW PRICED
220 NMR
Methacryloyl Chloride
SERVICE
95% and 99%
WRITE OR PHONE
MORGAN SCHAFFER CORP.
°
CH2=C-C-CI
ι
CH 3
Lee Pharmaceuticals
5110 Courtrai Ave., Montreal, Hue. (514) 731-4652
P.O. Box 3 8 3 6 , S. El Monte, CA. 9 1 7 3 3 ALLIED TRANSLATION SERVICE Patents»Scientific Literatures«Docu merits Specialities: Japanese, German, Chinese and French to English.
P.O. Box 10343, Jacksonville, Fla. 32207
INTERFACE
CO * All the Elements * Valence Shifts * Top 100 Angstroms
RESEARCH
ACETYLENIC CHEMICALS
ESCA * Fractions of a Monolayer * Surface Contaminants * Profiles of Multilayers
(415) 968-0375*P.O. Box 1088 Mtn View Ca 94040
|
Most complete single world's source. Some 500 derivatives. Hydrocar bons, acids, esters, ethers, ketones, alcohols etc. FARCHAN RES. LABS.
4702 E. 355 St., Willoughby, Ohio 44094
